Method for detecting aroma components of rose water, and method for determining the content of aroma components of rose water

Abstract

The present invention provides a method for detecting the aroma components of rose water and a method for determining the content of the aroma components of rose water, and belongs to the technical field of analysis and detection. The present invention adopts ultrasound-assisted dispersed liquid-liquid microextraction combined with gas chromatography-mass spectrometry to determine the aroma components of rose water, and can identify 80 aroma components from rose water, and can determine the content of 10 aroma components in rose water, and establish a simple, rapid and highly sensitive method for determining the aroma components of rose water, which can be used for the determination and analysis of large quantities of rose water samples.

Description

Technical Field

[0001] The invention relates to the technical field of analysis and detection, and in particular to a method for detecting aroma components of rose water and a method for determining the content of aroma components of rose water. Background Art

[0002] Rose water is a byproduct of rose essential oil during the distillation and extraction process. It is a pure natural product without any flavor or preservative. It contains trace amounts of rose essential oil and other water-soluble ingredients. It has a light and pleasant fragrance and has anti-allergic, anti-inflammatory, antibacterial, skin moisture replenishing, skin aging relief, and skin vitality enhancing effects. Rose flower cell fluid is a liquid condensed from volatile substances in rose flower cells under low temperature conditions, and has the natural fragrance of rose flowers. Rose water and rose flower cell fluid are collectively referred to as "rose water". Rose water is an important raw material for the development of rose series foods, cosmetics, and fresheners, and has a high development and utilization value. The aroma of rose water is an indicator that is focused on during product development and utilization. It is positively correlated with its quality and economic benefits, and is the main basis for determining the quality of rose water. Therefore, mastering the characteristic aroma components and content of rose water has important guiding significance for the rational processing and utilization of rose water. At present, there are several methods for enriching the aroma of rose water, including solid phase microextraction (SPME), purge and trap (P&T), liquid-liquid extraction (LLE) and activated carbon adsorption, but these methods all have certain limitations. For example, solid phase microextraction and purge and trap require special equipment, and the high equipment cost is not conducive to widespread application; liquid-liquid extraction usually consumes a large amount of organic solvents, which is harmful to human health and causes environmental pollution; activated carbon adsorption is time-consuming and has complicated steps, which is not conducive to batch testing. Summary of the invention

[0003] The object of the present invention is to provide a method for detecting rose water aroma components and a method for determining the content of rose water aroma components. The method can simultaneously detect 80 kinds of rose water aroma components and can achieve quantitative and accurate determination of 10 of the aroma components.

[0004] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0005] The present invention provides a method for detecting the aroma components of rose water, comprising the following steps:

[0006] Mixing rose water and a dispersive microextraction solution, and extracting under ultrasonic conditions to obtain an extract; the dispersive microextraction solution is a mixture of an extractant and a dispersant;

[0007] The extract is subjected to gas chromatography-mass spectrometry detection, and the obtained GC-MS spectrum is retrieved by using the NIST11 standard spectrum library to qualitatively identify the aroma components, thereby obtaining the aroma components of rose water;

[0008] The gas chromatography conditions in the gas chromatography-mass spectrometry detection include: chromatographic column: HP-INNOWAX; programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium; injection port temperature: 250°C; non-split injection;

[0009] The mass spectrometry conditions in the gas chromatography-mass spectrometry detection include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature 250°C; ion source temperature: 230°C; mass spectrometry voltage: 0.4kv; scanning mode: scan mode; mass scanning range: m / z35-500u;

[0010] The rose water aroma components include 2-heptanone, n-dodecane, isopentanol, 2,6,11-trimethyldodecane, 3-methyl-1,5-pentanediol, 2-ethyl-2-hexenal, cyclohexanone, 2-heptanol, methyl heptenone, n-hexanol, rose oxide A, rose oxide B, leaf alcohol, tetradecane, benzyl methyl ether, (S)-linalool oxide, n-heptanol, 6-methyl-5-heptene-2-ol, (E)-linalool oxide, benzaldehyde, linalool, dihydrocarveol, n-heneicosane , 4-terpene alcohol, myrcenol, (-)-trans-pine carveol, furfuryl alcohol, L-menthol, (Z)-3,7-dimethyl-2,6-octadienal, 2-(4-methyl-3-cyclohexenyl)propanal, α-terpineol, verbenol, benzyl acetate, citral, 3,7-dimethyl-7-octenol, citronellol, lavandulol, (-)-myrtenol, nerol, isogeraniol, caryophyllene oxide, phenylethyl acetate, verbenol, geraniol, guaiacol , benzyl alcohol, ocimene, isopulegol, phenylethyl alcohol, 3-(2,6,6-trimethyl-1-cyclohexen-1-yl) acrolein, 2,6-dimethyloct-7-ene-2,6-diol, perillyl alcohol, methyl eugenol, heptanoic acid, 4-tert-butylpropiophenone, 3-phenylpropanol, 4,8-dimethyl-3,7-nonadien-2-yl acetate, p-menthane-1,8-diol, 2,7-dimethyl-2,7-octanediol, 1-cyclohexyl-1-butanone, eucalyptol, Bisabolol oxide B, eugenol, hydroxycitronellol, elemenol, dec-7-en-2-one, isopulegol, cinnamyl alcohol, 2,4-di-tert-butylphenol, (R)-(+)-citronellal, farnesol, farnesic acid, neryl acetate, (2E)-3,7-dimethyl-2,6-octadienoic acid, 4-(2,2,6-trimethylcyclohexyl)-2-butanone, 3-ethoxy-3,7-dimethylocta-1,6-diene, elemenol, ceprene, bisabolol and benzoic acid.

[0011] Preferably, the volume ratio of the rose water to the dispersed microextraction solution is (5.0-7.0) mL: (600-800) μL.

[0012] Preferably, the extractant comprises dichloromethane; and the dispersant comprises acetonitrile.

[0013] Preferably, the volume ratio of the extractant to the dispersant is 1:(2-3).

[0014] Preferably, the extraction time is 1 to 3 minutes.

[0015] Preferably, the volume ratio of the rose water to the dispersed microextraction solution is 7.0 mL:600 μL; the volume ratio of the extractant to the dispersant is 1:2; and the extraction time is 3 min.

[0016] The present invention provides a method for determining the content of aroma components of rose water, comprising the following steps:

[0017] A standard series of 10 kinds of rose water aroma component mixed standard working solutions with different mass concentrations were prepared, and gas chromatography-mass spectrometry was performed to obtain the total ion current diagram of the standard substances of the 10 kinds of rose water aroma components, and a standard curve was established with the peak area as the ordinate and the mass concentration as the abscissa;

[0018] Mixing rose water and a dispersive microextraction solution, and extracting under ultrasonic conditions to obtain an extract; the dispersive microextraction solution is a mixture of an extractant and a dispersant;

[0019] The extract is subjected to gas chromatography-mass spectrometry detection, and the obtained GC-MS spectrum is compared with the spectrum of standard substances to determine 10 aroma components of rose water;

[0020] The gas chromatography conditions in the gas chromatography-mass spectrometry detection include: chromatographic column: HP-INNOWAX; programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium; injection port temperature: 250°C; split ratio: 50:1;

[0021] The mass spectrometry conditions in the gas chromatography-mass spectrometry detection include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature 250°C; ion source temperature: 230°C; mass spectrometry voltage: 0.4kv; scanning mode: scan mode; mass scanning range: m / z35-500u;

[0022] The peak areas of the spectra obtained from the 10 aroma components of the rose water are compared with the standard curve to obtain the contents of the aroma components of the rose water;

[0023] The 10 rose water aroma components include citronellol, linalool, citronellyl acetate, methyl eugenol, phenylethyl alcohol, geraniol acetate, nerol, eugenol, geraniol and benzyl alcohol.

[0024] The present invention provides a method for detecting aroma components of rose water. The present invention adopts ultrasound-assisted dispersed liquid-liquid microextraction combined with gas chromatography-mass spectrometry technology to determine the aroma components of rose water. The dispersed liquid-liquid microextraction uses an extractant to form dispersed fine droplets in a sample solution under the action of a dispersant, forming an extractant-dispersant-sample solution three-phase emulsion system, which can increase the contact area between the extractant and the analyte, so that the analyte can quickly reach a distribution equilibrium between the sample solution and the extractant to complete the extraction. The present invention is the first to use liquid-liquid microextraction technology for the extraction of aroma components of rose water, which has the advantages of simple operation, low cost, high enrichment multiple and good reproducibility, and can be used for the determination and analysis of large quantities of rose water samples.

[0025] The method of the present invention can identify 80 aroma components from rose water, among which 61 aroma components are identified from rose cell sap, 55 aroma components from rose water, 53 aroma components from fresh rose water, and 55 aroma components from pickled rose water. The aroma components with relatively high content include citronellol, hydroxycitronellol, eugenol, linalool, α-terpineol, phenylethyl alcohol, nerol, geraniol, methyl eugenol, etc. The results of the embodiment show that the aroma component analysis of fresh rose cell sap and rose water, rose water obtained by different processing techniques, and rose water from different manufacturers are different in their relative content and composition, which provides a certain theoretical basis for the aroma characteristics of rose water and its development and utilization.

[0026] The invention provides a method for determining the content of rose water aroma components. The invention adopts ultrasound-assisted dispersed liquid-liquid microextraction-gas chromatography / mass spectrometry technology to quickly quantify the rose water aroma components, and can determine the contents of 10 aroma components in rose water, and establish a simple, rapid and highly sensitive rose water aroma component determination method. Moreover, the 10 aroma components in rose water have a good linear relationship within a certain mass concentration range, and the correlation coefficient is greater than 0.9991. The method detection limit is 0.050-0.078 mg / L, the quantitative lower limit is 0.166-0.261 mg / L, the average recovery rate is 79.806%-113.780%, and the relative standard deviation is 2.016%-9.576%. The method is accurate and reliable, has the advantages of simple operation, small amount of organic solvent, rapidity and sensitivity, and can be used for the determination and analysis of large quantities of rose water samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The effect of different sample amounts on the enrichment efficiency of aroma components;

[0028] Figure 2 The effect of different ultrasonic extraction time on the enrichment efficiency of aroma components;

[0029] Figure 3 The effects of different extractant types (a) and extractant volumes (b) on the enrichment efficiency of aroma components;

[0030] Figure 4 The effects of dispersant types and the volume ratio of extractant to dispersant on the enrichment efficiency of aroma components;

[0031] Figure 5 is the total ion current diagram of the aroma components of rose water in Example 1; a is the total ion current diagram of rose fresh flower cell fluid, b is the total ion current diagram of rose water, c is the total ion current diagram of fresh flower water, and d is the total ion current diagram of pickled flower water;

[0032] Figure 6 This is a classification analysis diagram of the aroma components of rose flower cell fluid and rose water;

[0033] Figure 7 This is a classification analysis chart of the aroma components of rose water with different processing techniques;

[0034] Figure 8 This is a classification chart of the aroma components of rose water from different manufacturers;

[0035] Fig. 9 The total ion current diagram of 10 characteristic aroma component standard substances;

[0036] Fig.10 : The total ion current diagram of the rose dew aroma component in Example 10, a is the total ion current diagram of the rose fresh flower cell sap (split ratio: 50:1), b is the total ion current diagram of rose water (split ratio: 50:1), c is the total ion current diagram of fresh flower water (split ratio: 50:1), and d is the total ion current diagram of pickled flower water (split ratio: 50:1). DETAILED DESCRIPTION

[0037] The present invention provides a method for detecting the aroma components of rose water, comprising the following steps:

[0038] Mixing rose water and a dispersive microextraction solution, and extracting under ultrasonic conditions to obtain an extract; the dispersive microextraction solution is a mixture of an extractant and a dispersant;

[0039] The extract is subjected to gas chromatography-mass spectrometry detection, and the obtained GC-MS spectrum is retrieved by using the NIST11 standard spectrum library to qualitatively identify the aroma components, thereby obtaining the aroma components of rose water;

[0040] The gas chromatography conditions in the gas chromatography-mass spectrometry detection include: chromatographic column: HP-INNOWAX; programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium; injection port temperature: 250°C; non-split injection;

[0041] The mass spectrometry conditions in the gas chromatography-mass spectrometry detection include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature 250°C; ion source temperature: 230°C; mass spectrometry voltage: 0.4kv; scanning mode: scan mode; mass scanning range: m / z35-500u;

[0042] The rose water aroma components include 2-heptanone, n-dodecane, isopentanol, 2,6,11-trimethyldodecane, 3-methyl-1,5-pentanediol, 2-ethyl-2-hexenal, cyclohexanone, 2-heptanol, methyl heptenone, n-hexanol, rose oxide A, rose oxide B, leaf alcohol, tetradecane, benzyl methyl ether, (S)-linalool oxide, n-heptanol, 6-methyl-5-heptene-2-ol, (E)-linalool oxide, benzaldehyde, linalool, dihydrocarveol, n-heneicosane , 4-terpene alcohol, myrcenol, (-)-trans-pine carveol, furfuryl alcohol, L-menthol, (Z)-3,7-dimethyl-2,6-octadienal, 2-(4-methyl-3-cyclohexenyl)propanal, α-terpineol, verbenol, benzyl acetate, citral, 3,7-dimethyl-7-octenol, citronellol, lavandulol, (-)-myrtenol, nerol, isogeraniol, caryophyllene oxide, phenylethyl acetate, verbenol, geraniol, guaiacol , benzyl alcohol, ocimene, isopulegol, phenylethyl alcohol, 3-(2,6,6-trimethyl-1-cyclohexen-1-yl) acrolein, 2,6-dimethyloct-7-ene-2,6-diol, perillyl alcohol, methyl eugenol, heptanoic acid, 4-tert-butylpropiophenone, 3-phenylpropanol, 4,8-dimethyl-3,7-nonadien-2-yl acetate, p-menthane-1,8-diol, 2,7-dimethyl-2,7-octanediol, 1-cyclohexyl-1-butanone, eucalyptol, Bisabolol oxide B, eugenol, hydroxycitronellol, elemenol, dec-7-en-2-one, isopulegol, cinnamyl alcohol, 2,4-di-tert-butylphenol, (R)-(+)-citronellal, farnesol, farnesic acid, neryl acetate, (2E)-3,7-dimethyl-2,6-octadienoic acid, 4-(2,2,6-trimethylcyclohexyl)-2-butanone, 3-ethoxy-3,7-dimethylocta-1,6-diene, elemenol, ceprene, bisabolol and benzoic acid.

[0043] In the present invention, unless otherwise specified, the required reagents or instruments are commercially available products well known to those skilled in the art.

[0044] In the present invention, the rose water preferably includes one or more of rose fresh flower cell fluid, rose water, fresh rose flower water and rose pickled flower water. The present invention has no special limitation on the source of the rose water, and commercially available products known in the art can be used; in the embodiments of the present invention, the rose fresh flower water and rose pickled flower water samples are provided by Gansu Dongfang Tianrun Rose Industry Company; the rose water and rose fresh flower cell fluid samples are provided by Gansu Changsheng Rose Development Co., Ltd.

[0045] In the present invention, the dispersed microextraction solution is a mixture of an extractant and a dispersant; the extractant preferably includes dichloromethane; the dispersant preferably includes acetonitrile; the volume ratio of the extractant to the dispersant is preferably 1:(2-3), more preferably 1:2; the volume ratio of the rose water to the dispersed microextraction solution is preferably (5.0-7.0) mL:(600-800) μL, more preferably 7.0 mL:600 μL.

[0046] The present invention has no special limitation on the mixing of the rose water and the dispersed microextraction solution, and the materials can be mixed evenly according to a process well known in the art.

[0047] The present invention has no particular limitation on the method of providing the ultrasonic condition, and any ultrasonic instrument known in the art can be used; the extraction time is preferably 1 to 3 minutes, more preferably 3 minutes.

[0048] After the extraction is completed, the present invention preferably centrifuges the obtained mixture at a speed of 3000 r / min for 3 minutes. The obtained extract phase is deposited at the bottom of the tube and has a clear boundary with the aqueous phase. The extract phase is completely sucked out using a microsyringe to obtain an extract.

[0049] After obtaining the extract, the present invention performs gas chromatography-mass spectrometry on the extract, and uses the obtained GC-MS spectrum to search the NIST11 standard spectrum library to qualitatively identify the aroma components, thereby obtaining the rose water aroma components.

[0050] In the present invention, the conditions of gas chromatography in the gas chromatography-mass spectrometry detection include: chromatographic column: HP-INNOWAX (60m×0.250mm×0.5μm); programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium (purity ≥99.999%); injection port temperature: 250°C; non-split injection.

[0051] In the present invention, the mass spectrometry conditions in the gas chromatography-mass spectrometry detection include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature 250°C; ion source temperature: 230°C; mass spectrometry voltage: 0.4kv; scanning mode: scan mode; mass scanning range: m / z35~500u.

[0052] In the present invention, the gas chromatography-mass spectrometry detection is preferably performed by GCMS-QP2010Ultra gas chromatography / mass spectrometry (Shimadzu Corporation, Japan).

[0053] In the present invention, the rose water aroma components in the GC-MS spectrum are preferably searched using the NIST17 standard spectral library, and the identification components with a matching degree greater than 85 (maximum value is 100) are reported and confirmed in combination with standard substances.

[0054] In the present invention, the rose water aroma components include 2-heptanone, n-dodecane, isopentanol, 2,6,11-trimethyldodecane, 3-methyl-1,5-pentanediol, 2-ethyl-2-hexenal, cyclohexanone, 2-heptanol, methyl heptenone, n-hexanol, rose oxide A, rose oxide B, leaf alcohol, tetradecane, benzyl methyl ether, (S)-linalool oxide, n-heptanol, 6-methyl-5-heptene-2-ol, (E)-linalool oxide, benzaldehyde, linalool, dihydrocarveol, n-Hexedan, 4-terpene alcohol, myrcenol, (-)-trans-pine carveol, furfuryl alcohol, L-menthol, (Z)-3,7-dimethyl-2,6-octadienal, 2-(4-methyl-3-cyclohexenyl)propanal, α-terpineol, verbenol, benzyl acetate, citral, 3,7-dimethyl-7-octenol, citronellol, lavandinol, (-)-myrtenol, nerol, isogeraniol, caryophyllene oxide, phenylethyl acetate, verbenol, geraniol, guaiac Benzyl alcohol, ocimene, isopulegol, phenylethyl alcohol, 3-(2,6,6-trimethyl-1-cyclohexen-1-yl) acrolein, 2,6-dimethyloct-7-ene-2,6-diol, perillyl alcohol, methyl eugenol, heptanoic acid, 4-tert-butylpropiophenone, 3-phenylpropanol, 4,8-dimethyl-3,7-nonadien-2-yl acetate, p-menthane-1,8-diol, 2,7-dimethyl-2,7-octanediol, 1-cyclohexyl-1-butanone, eucalyptene alcohol, bisabolol oxide B, eugenol, hydroxycitronellol, elemenol, dec-7-en-2-one, isopulegol, cinnamyl alcohol, 2,4-di-tert-butylphenol, (R)-(+)-citronellal acid, farnesol, farnesic acid, neryl acetate, (2E)-3,7-dimethyl-2,6-octadienoic acid, 4-(2,2,6-trimethylcyclohexyl)-2-butanone, 3-ethoxy-3,7-dimethylocta-1,6-diene, elemenol, ceprene, bisabolol and benzoic acid.

[0055] The present invention provides a method for determining the content of aroma components of rose water, comprising the following steps:

[0056] A standard series of 10 kinds of rose water aroma component mixed standard working solutions with different mass concentrations were prepared, and gas chromatography-mass spectrometry was performed to obtain the total ion current diagram of the standard substances of the 10 kinds of rose water aroma components, and a standard curve was established with the peak area as the ordinate and the mass concentration as the abscissa;

[0057] Mixing rose water and a dispersive microextraction solution, and extracting under ultrasonic conditions to obtain an extract; the dispersive microextraction solution is a mixture of an extractant and a dispersant;

[0058] The extract is subjected to gas chromatography-mass spectrometry detection, and the obtained GC-MS spectrum is compared with the spectrum of standard substances to determine 10 aroma components of rose water;

[0059] The gas chromatography conditions in the gas chromatography-mass spectrometry detection include: chromatographic column: HP-INNOWAX; programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium; injection port temperature: 250°C; split ratio: 50:1;

[0060] The mass spectrometry conditions in the gas chromatography-mass spectrometry detection include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature 250°C; ion source temperature: 230°C; mass spectrometry voltage: 0.4kv; scanning mode: scan mode; mass scanning range: m / z35-500u;

[0061] The peak areas of the spectra obtained from the 10 aroma components of the rose water are compared with the standard curve to obtain the content of the aroma components of the rose water;

[0062] The 10 rose water aroma components include citronellol, linalool, citronellyl acetate, methyl eugenol, phenylethyl alcohol, geraniol acetate, nerol, eugenol, geraniol and benzyl alcohol.

[0063] In the present invention, the process of preparing a standard series of 10 rose water aroma component mixed standard working solutions with different mass concentrations is preferably:

[0064] 1) Standard mixed stock solution I and standard series mixed working solution

[0065] Using dichloromethane as solvent, accurately weigh appropriate amounts of linalool, citronellyl acetate, geranyl acetate, citronellol, nerol, geraniol, benzyl alcohol, phenylethyl alcohol, methyl eugenol, and eugenol standards (accurate to 0.1 mg), and dilute to 25 mL with dichloromethane to prepare mass concentrations of 2000 mg / L, 4340 mg / L, 4788 mg / L, 3632 mg / L, 2572 mg / L, and 4536 mg / L, respectively. , 4120 mg / L, 4496 mg / L, 4864 mg / L, and 5720 mg / L single standard solutions, accurately measure 750 μL, 400 μL, 400 μL, 400 μL, 750 μL, 400 μL, 400 μL, 400 μL, 400 μL, 400 μL, and 400 μL of the above single standard solutions in a 5 mL volumetric flask to make up to volume to prepare standard mixed stock solution I. The mass concentration of the standard mixed stock solution I is shown in Table 2.

[0066] 2) Using dichloromethane as solvent, dilute the standard mixed stock solution I step by step.

[0067] Take 700 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 1; take 500 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 2; take 350 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 3; take 170 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 4; take 70 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 5; take 20 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 6; take 10 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 6.

[0068] In the present invention, the gas chromatography conditions in the gas chromatography-mass spectrometry detection preferably include: chromatographic column: HP-INNOWAX; programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium; inlet temperature: 250°C; split ratio: 50:1.

[0069] In the present invention, the mass spectrometry conditions in the gas chromatography-mass spectrometry detection preferably include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature 250°C; ion source temperature: 230°C; mass spectrometry voltage: 0.4kv; scanning mode: scan mode; mass scanning range: m / z35~500u.

[0070] The present invention has no particular limitation on the process of establishing the standard curve. The standard curve can be established by using standard mixed working solutions of different concentrations according to a process well known in the art, with the peak area as the ordinate and the mass concentration as the abscissa.

[0071] The present invention has no special limitation on the process of comparing the peak area of ​​the spectrum obtained by the above technical solution with the standard curve to measure the content of the aroma components of rose water, and can be carried out according to the process well known in the art.

[0072] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0073] In the following examples, the samples used were: rose fresh flower cell fluid, rose water, rose fresh flower water and rose pickled flower water;

[0074] Pickled rose floral water is obtained by extracting rose essential oil from fresh flowers through salt pickling, and fresh rose floral water is obtained by extracting rose essential oil from fresh flowers without salt pickling. The samples of pickled rose floral water and fresh rose floral water are provided by Gansu Oriental Tianrun Rose Industry Co., Ltd.; rose floral water is obtained by extracting rose essential oil from fresh flowers through salt pickling, and the samples are provided by Gansu Changsheng Rose Development Co., Ltd.; rose flower cell fluid is a liquid formed by condensation of volatile substances in rose flower cells under low temperature conditions, and the samples of rose flower cell fluid are provided by Gansu Changsheng Rose Development Co., Ltd.

[0075] Example 1

[0076] 7.0 mL of rose samples (rose fresh cell fluid, rose water, fresh rose water and rose pickled water) were respectively transferred into 15 mL conical bottom centrifuge tubes with stoppers, 600 μL of dispersive microextraction solution (the volume ratio of dichloromethane (extractant) to acetonitrile (dispersant) was 1:2) was added, and extraction was performed in an ultrasonic instrument for 3 min. The obtained mixture was centrifuged at 3000 r / min for 3 min. The obtained extract phase was deposited at the bottom of the centrifuge tube. The enriched extract phase deposited at the bottom of the tube was completely sucked out with a microsyringe to obtain an extract;

[0077] The extract was subjected to gas chromatography-mass spectrometry detection in a GCMS-QP2010Ultra gas chromatograph / mass spectrometer:

[0078] Gas chromatography conditions: chromatographic column: HP-INNOWAX (60m×0.250mm×0.5μm); programmed temperature: initial temperature 60°C, maintained for 1 minute, increased to 245°C / min at a rate of 2°C / min, maintained for 5 minutes; carrier gas: high-purity helium (purity ≥99.999%); injection port temperature: 250°C; splitless injection;

[0079] Mass spectrometry conditions: electron bombardment ion source; electron energy: 70 eV; mass spectrometry voltage: 0.4 kV; transmission line temperature 250 ° C; ion source temperature: 230 ° C; mass spectrometry voltage: 0.4 kV; scanning mode: scan mode; mass scanning range: m / z35-500u;

[0080] The obtained spectra were searched using the NIST17 standard spectral library, and the identification components with a matching degree greater than 85 (maximum value is 100) were reported and confirmed in combination with standard substances.

[0081] Example 2

[0082] The only difference from Example 1 is that the sample amounts are 1.0 mL, 3.0 mL, 5.0 mL, 9.0 mL, and 11.0 mL, respectively.

[0083] Example 3

[0084] The only difference from Example 1 is that the extraction time is 0 min, 1 min, 5 min, 7 min, and 9 min.

[0085] Example 4

[0086] The only difference from Example 1 is that the extracting agents are chloroform, chlorobenzene, carbon tetrachloride and toluene, respectively.

[0087] Example 5

[0088] The only difference from Example 1 is that the volumes of the extractants are 50 μL, 100 μL, 150 μL, and 250 μL, respectively.

[0089] Example 6

[0090] The only difference from Example 1 is that the dispersant is methanol or acetone.

[0091] Example 7

[0092] The only difference from Example 1 is that the volume ratio of the extractant to the dispersant is 1:3, 1:4, 1:5, 1:6, 1:7 or 1:8.

[0093] Example 8

[0094] The only difference from Example 1 is that the chromatographic columns are HP-5MS (30m×0.250mm×0.25μm) or DB-FFAP (60m×0.250mm×0.5μm).

[0095] Example 9

[0096] The only difference from Example 1 is that the mass spectrometer voltages are 0.3 kv, 0.5 kv and 0.6 kv respectively.

[0097] Example 10

[0098] The only difference from Example 1 is that the chromatographic detection adopts split injection with a split ratio of 50:1.

[0099] 1. Test Results

[0100] 1) Figure 1 The effect of different sample amounts on the enrichment efficiency of rose water aroma components; Figure 1 It can be seen that when the sample volume is 1.0mL and 3.0mL, there is an obvious stratification phenomenon between the rose water sample and the supernatant (acetonitrile), but there is no stratification between dichloromethane and the sample solution. When the supernatant is analyzed, only citronellol is detected, and other major aroma components are not detected; when the sample volume is 5mL, 7mL, 9mL, and 11mL, dichloromethane and the rose water sample form a stable two-phase system with a clear stratification interface, but the volume of dichloromethane in the precipitation layer is inversely proportional to the sample volume. The larger the sample volume, the smaller the volume of the lower precipitant; when the sample volume is 9.0mL, the precipitant volume is less than 20μL, and the precipitant volume is even less when the sample volume is 11.0mL. The precipitant volume fails to reach the minimum volume required for automatic injection of the gas chromatography-mass spectrometry instrument, and manual injection analysis is required. It is not suitable for high-throughput sample determination. The optimization results are as follows Figure 1 As shown in the figure, as the sample volume increases, the peak area and the number of peaks both show an upward trend, and the peak area and the number of peaks are the highest when the sample volume is 11 mL. However, since the mass spectra of the characteristic components of rose water, linalool, citronellol, nerol, geraniol, and eugenol, are saturated when the sample volume is 9.0 mL and 11.0 mL, the accuracy of quantification is affected.

[0101] Figure 2 The effect of different ultrasonic extraction times on the enrichment efficiency of rose water aroma components was investigated. Figure 2 It can be seen that the total peak area and the number of peaks showed a trend of first increasing and then decreasing. When the ultrasonic time was 3 minutes, the total peak area and the number of peaks reached the highest, so 3 minutes was selected as the optimal ultrasonic time in the experiment.

[0102] Figure 3 The effects of different extractants on the enrichment efficiency of rose water aroma components are shown in Figure 2. Figure 3As shown, when dichloromethane is used as the extractant, the total peak area and peak number of the aroma components are the highest, and the enrichment efficiency of the aroma components of rose water is higher; when toluene is used as the extractant, toluene and the rose water sample cannot form a two-phase system; therefore, dichloromethane is selected as the extractant.

[0103] The effect of the volume of the extractant on the enrichment efficiency of aroma components was studied. The results showed that when the extractant was taken at 50μL, 100μL, and 150μL, respectively, dichloromethane and rose water samples could not form a stable two-phase system; when the extractant was taken at 200μL and 250μL, the interface between dichloromethane and rose water samples was clear after centrifugation. Considering the enrichment multiple and reagent dosage, the dichloromethane dosage of 200μL was selected in this experiment.

[0104] Figure 4 The effects of the type of dispersant and the volume ratio of the extractant to the dispersant on the enrichment efficiency of the aroma components of rose water are: Figure 4 From a, we can see that the extraction efficiency of acetonitrile as a dispersant is higher than that of acetone and methanol, and the total peak area and peak number of its aroma components are higher. Figure 4 As shown in Figure b, the total peak area and peak number of rose water aroma components are the highest when the volume ratio of the two is 1:2, and the extraction ability is stronger. Therefore, the volume ratio of dichloromethane and acetonitrile is 1:2.

[0105] Comparison of the results of Example 8 with those of Example 1 shows that the separation effect of HP-5MS is not good. After verification by standard substances, the chromatographic peaks of citronellol and nerol, the main aroma components of rose water, completely overlap; HP-INNOWAX and DB-FFAP can both achieve good separation effects, but under the same integration event, the peak area and peak number of DB-FFAP are lower than those of HP-INNOWAX. The content of the main aroma components of rose water is inconsistent. In order to detect trace aroma components as much as possible and improve the sensitivity of the equipment, the non-split injection mode is adopted.

[0106] Comparison of the results of Example 9 with those of Example 1 shows that at 0.3 kv, the chromatographic peak response of the main aroma components is relatively low, only linalool and citronellol are detected, and other components are not detected; at 0.4 kv, 0.5 kv, and 0.6 kv, the main aroma components can all be detected; under the conditions of 0.5 kv and 0.6 kv, the chromatographic peaks of the main aroma components are oversaturated, and the peak shapes of each peak are not sharp, especially the chromatographic peak of citronellol is wide and asymmetric, which is not conducive to quantitative analysis. In addition, the baseline is unstable and the interference of miscellaneous peaks is large, so the analysis is selected at 0.4 kv.

[0107] 2. Qualitative Testing

[0108] 1) After the rose water aroma components were separated by GC-MS in Example 1, the total ion current diagram of the rose water aroma components obtained was shown in Figure 5, where a is the total ion current of rose flower cell fluid, b is the total ion current of rose water, c is the total ion current of fresh flower water, and d is the total ion current of pickled flower water. The spectrum was searched using the NIST17 standard spectral library, and the identification components with a matching degree greater than 85 (maximum value is 100) were reported. The qualitative results of the aroma components of rose water were obtained by combining with the standard substance confirmation, and the peak area normalization method was used for relative quantification. The qualitative results and relative contents are shown in Table 1.

[0109] Table 1 Identification results and relative contents of rose water aroma components

[0110]

[0111]

[0112]

[0113]

[0114] Note: Nd means not detected.

[0115] As shown in Table 1, a total of 80 aroma components were identified in different rose dews, including 61 in rose cell sap, 55 in rose water, 53 in fresh rose water and 55 in pickled rose water. The aroma components with relatively high content include citronellol (10.22%-30.09%), hydroxycitronellol (2.14%-10.23%), eugenol (6.75%-9.76%), linalool (4.96%-14.29%), α-terpineol (2.38%-10.97%), phenylethanol (3.84%-5.96%), nerol (0.25%-6.73%), geraniol (1.27%-14.68%), methyl eugenol (2.30%-5.93%), etc. According to the different functional groups, they can be divided into 8 major categories of substances, namely: alcohols, phenols, ethers, ketones, esters, aldehydes, acids, and others.

[0116] 2) Analysis of aroma components of rose flower cell fluid and rose water

[0117] Rose flower cell sap is a liquid formed by condensation of volatile substances in rose flower cells under low temperature conditions, and has the natural fragrance of rose flowers. Rose water is a byproduct produced during the distillation and extraction process of rose essential oil. The aroma components of rose flower cell sap are detected according to the method of Example 1. The classification diagram of the aroma components of rose flower cell sap and rose water is shown in Figure 6 .

[0118] Figure 6 This is a classification analysis diagram of the aroma components of rose flower cell fluid and rose water. Figure 6It can be seen that a total of 70 aroma components were identified in rose flower cell sap and rose water, of which 61 were identified in rose flower cell sap and 55 were identified in rose water. The common components of the two include 45 such as citronellol, nerol, geraniol, and phenylethanol, and the sum of the relative contents are 93.14% and 85.98% respectively; the specific components of rose flower cell sap include 16 such as neryl acetate, benzyl acetate, benzaldehyde, and citral, with a relative total content of 1.89%; the specific components of rose water include 10 such as ocimene, (E)-linalool oxide, isopentanol, and myrcenol, with a relative total content of 4.17%.

[0119] Depend on Figure 6 It can be seen that the relative content of alcohol compounds in rose flower cell sap and rose water is relatively high, with a total of 39 species identified, of which 33 species were identified in rose flower cell sap and 32 species were identified in rose water. The content of alcohol substances in rose flower cell sap (relative content sum 79.35%) is significantly higher than that in rose water (relative content sum 66.37%). The content of phenolic substances in rose flower cell sap and rose water is quite different, with the relative content sum being 7.07% and 9.89% respectively. A total of 4 ether substances were identified in rose flower cell sap and rose water, with the relative content sum being 4.63% and 7.45% respectively. The unique component of rose flower cell sap is rose ether B (0.05%). 5 ketone substances were identified, with the relative content sum being 0.82% and 2.12% in rose flower cell sap and rose water respectively. Three esters were identified in rose flower cell sap and rose water, of which rose water had benzyl acetate (0.17%), neryl acetate (0.11%), and phenylethyl acetate (0.25%). Three aldehydes were found in rose flower cell sap, with a relative content of 0.17%, and two aldehydes were found in rose water, with a relative content of 0.54%. Three acids were identified, including (R)-(+)-citronellal acid (0.28%) and (2E)-3,7-dimethyl-2,6-octadienoic acid (0.25%), and heptanoic acid (0.82%). In addition, nine other compounds were identified, with relative contents of 1.86% and 2.82% in rose flower cell sap and rose water, respectively. Through the above discussion and analysis, the aroma components of rose water and rose flower cell sap differ in their relative content and composition.

[0120] 3) Analysis of aroma components of rose water obtained by different processing techniques

[0121] Rose water is a byproduct produced during the distillation and extraction of rose essential oil. The distillation and extraction process of rose essential oil is divided into two types: direct extraction from fresh flowers and extraction from fresh flowers pickled. The rose water (fresh flower water and pickled flower water) produced by the two extraction processes was extracted and tested for its aroma components according to the method of Example 1. The classification diagram of the obtained aroma components is shown in FIG. Figure 7 shown.

[0122] Figure 7 This is a classification analysis of the aroma components of rose water with different processing techniques. Figure 7 It can be seen that a total of 62 aroma components were identified in fresh flower water and pickled flower water, of which 53 were identified in fresh flower water and 55 in pickled flower water. The total components included 46 components such as citronellol, nerol, geraniol, and phenylethyl alcohol, and the sum of the relative contents in fresh flower water and pickled flower water were 92.84% and 87.25%, respectively; the unique components of fresh flower water included 7 components such as dihydrocarveol, 4-terpenol, (-)-trans-monopilenol, with a relative total content of 0.97%; the unique components of pickled flower water included 9 components such as benzyl ether, furfuryl alcohol, isopulegol, and benzoic acid, with a relative total content of 5.71%.

[0123] A total of 33 alcohol compounds were identified in fresh flower water and pickled flower water, with the relative contents of 76.05% and 66.85% respectively. Alcohol compounds are the main aroma components of roses, and the content of such compounds determines the quality of rose water. Citronellol has a sweet rose fragrance, linalool has a green tea fragrance, and phenylethanol has a sweet honey flavor, which is the main source of rose aroma in rose water. Fresh flower water has four unique types of dihydrocarveol (0.08%), 4-terpene alcohol (0.13%), L-menthol (0.13%), (-)-trans-pine carveol (0.15%), and pickled flower water has four unique types of furfuryl alcohol (0.12%), isopulegol (0.15%), 2,7-dimethyl-2,7-octanediol (0.11%), and bisabolol (0.11%). Pickled flower water contains 1 ether (0.15%), 2 acids (2.59%) and 2 ketones (2.48%); fresh flower water contains 2 aldehydes (0.41%) and 1 ester (0.07%); in addition to the above substances, 7 other types of compounds were also identified, with relative contents of 2.57% and 2.90% in fresh flower water and pickled flower water, respectively.

[0124] 4) Analysis of aroma components of rose water from different manufacturers

[0125] The unique fragrance of rose water is dominated by one or several aroma components, and the rest play a coordinating role. Due to the different proportions of various components, different fragrances are exhibited. The classification chart of the aroma components of rose water from different manufacturers is shown in Figure 8 Based on the data analysis of rose water (manufacturer 1) and salted floral water (manufacturer 2) in Table 1, the aroma component composition of rose water from different manufacturers was explored. The aroma component classification diagram is shown in Figure 8As shown. A total of 68 aroma components were identified in the rose water of manufacturer 1 and manufacturer 2, of which 55 were identified in both manufacturer 1 and manufacturer 2. As shown in Table 1, there are differences in the types and contents of rose water (manufacturer 1) and salted flower water (manufacturer 2). The common components of the two include 42 components such as citronellol, nerol, eugenol, methyl eugenol, etc., and the sum of the relative contents in manufacturer 1 and manufacturer 2 are 75.81% and 88.01%, respectively; the unique components of rose water of manufacturer 1 include ocimene, 1-cyclohexyl-1-butanone, cinnamyl alcohol, 2-ethyl-2-hexenal, benzyl alcohol, etc., with a relative total content of 13.34%; the unique components of pickled flower water include guaiacol, farnesol, benzyl methyl ether, lavender alcohol, citral, benzyl acetate, (R)-(+)-citronellal, benzoic acid, etc., with a relative total content of 4.95%.

[0126] The content of alcohol compounds in rose water is significantly higher than other compounds. A total of 35 alcohol compounds were identified, 32 of which were identified by manufacturer 1 and 29 by manufacturer 2, with relative contents of 66.37% and 66.85% respectively. The main alcohol substances are citronellol, hydroxycitronellol, linalool, α-terpineol, phenylethyl alcohol, etc. These compounds have a positive contribution to the aroma characteristics of rose water. Ketones, aldehydes, esters and ethers are also important components of the aroma components of rose water. Ketone substances in rose water from different manufacturers vary significantly, with relative total contents of 2.12% and 3.37% respectively. These components make rose water have oily smell. The rose water from manufacturer 1 has 1-cyclohexyl-1-butanone (0.11%), and the rose water from manufacturer 2 has 4-tert-butylphenylacetone (0.16%) and dec-7-en-2-one (0.21%). The types and contents of aldehydes in rose water from different manufacturers were different. Three aldehydes were found in rose water from manufacturer 1, with a total relative content of 0.68%; one aldehyde was identified from manufacturer 2, with a relative content of 0.19%. Two esters were identified in rose water from manufacturer 2, with a relative content of 0.50%. A total of four acids were identified, with one specific heptanoic acid (0.82%) from manufacturer 1 and three specific (R)-(+)-citronellal acid (0.72%), farnesic acid (0.13%), and benzoic acid (2.46%) from manufacturer 2. Four ether substances were identified in rose water, and the relative contents were 7.45% and 7.02% respectively. Among them, benzyl ether (0.15%) was unique to manufacturer 2. Rose ether was identified in rose water from different manufacturers. Since it was difficult to distinguish the left-handed rose ether and the right-handed rose ether, it was temporarily identified as rose ether A. Rose ether has a sweet green floral aroma, and the diluted rose ether has the aroma of roses and fresh bay leaves. (+)-rose ether has a sweet and delicate aroma, and (-)-rose ether is green. The left-handed aroma is sweeter than the right-handed aroma, and the right-handed aroma has a slightly spicy aroma. In addition, phenols and other compounds are also indispensable components of the aroma of rose water. Guaiacol (0.08%) is unique to manufacturer 2, and ocimene (0.10%) is unique to manufacturer 1. Ocimene has a grassy and floral aroma accompanied by the aroma of neroli. The above discussion shows that the contributions of alcohols, ketones, aldehydes, esters, phenols, ethers, acids and other types in rose water from different manufacturers are different.

[0127] 3. Quantitative Testing

[0128] 1.1) Standard mixed stock solution I and standard series mixed working solution

[0129] Using dichloromethane as solvent, accurately weigh appropriate amounts of linalool, citronellyl acetate, geranyl acetate, citronellol, nerol, geraniol, benzyl alcohol, phenylethyl alcohol, methyl eugenol, and eugenol standards (accurate to 0.1 mg), and dilute to 25 mL with dichloromethane to prepare mass concentrations of 2000 mg / L, 4340 mg / L, 4788 mg / L, 3632 mg / L, 2572 mg / L, and 4536 mg / L, respectively. , 4120 mg / L, 4496 mg / L, 4864 mg / L, and 5720 mg / L single standard solutions, accurately measure 750 μL, 400 μL, 400 μL, 400 μL, 750 μL, 400 μL, 400 μL, 400 μL, 400 μL, 400 μL, and 400 μL of the above single standard solutions in a 5 mL volumetric flask to make up to volume to prepare standard mixed stock solution I. The mass concentration of the standard mixed stock solution I is shown in Table 2.

[0130] Using dichloromethane as solvent, dilute the standard mixed stock solution I step by step.

[0131] Take 700 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 1; take 500 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 2; take 350 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 3; take 170 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 4; take 70 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 5; take 20 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 6; take 10 μL of standard mixed stock solution I, make the volume to 1.0 mL, and prepare standard mixed working solution 6; the mass concentrations of the standard series mixed working solutions are shown in Table 2.

[0132] Table 2 Standard series mixed working solution concentration (mg / L)

[0133]

[0134]

[0135] 2) Standard mixed stock solution II and standard mixed stock solution III

[0136] With anhydrous ethanol as solvent, accurately weigh appropriate amounts of linalool, citronellyl acetate, geranyl acetate, citronellol, nerol, geraniol, benzyl alcohol, phenylethyl alcohol, methyl eugenol, and eugenol standards (accurate to 0.1 mg), dissolve them in anhydrous ethanol and make up to 25 mL, and prepare the mass concentrations to be 3352 mg / L, 4645 mg / L, 4511 mg / L, 4180 mg / L, 4332 mg / L, 4351 mg / L, 4445 mg / L, 4226 mg / L, 4286 mg / L, and 4226 mg / L, respectively. 0 mg / L standard mixed stock solution II; take 40 μL of standard mixed stock solution II, dilute to 1.0 mL with anhydrous ethanol to prepare standard mixed stock solutions III with mass concentrations of 134.08 mg / L, 185.80 mg / L, 180.44 mg / L, 167.20 mg / L, 173.28 mg / L, 174.04 mg / L, 177.80 mg / L, 169.04 mg / L, 171.44 mg / L, and 168.80 mg / L for addition recovery experiments.

[0137] 2. Standard curve, method detection limit and quantitative lower limit

[0138] After preparing the standard series mixed standard working solution, gas chromatography-mass spectrometry was performed according to the method of Example 10, and the total ion current diagram of the standard substances of the 10 aroma components was shown in FIG. Fig. 9 ; A standard curve was drawn using peak area (Y) versus mass concentration (X, mg / L) and regression calculation was performed. The results are shown in Table 3.

[0139] Table 3 Linear relationships, detection limits and quantification limits of 10 characteristic aroma components

[0140]

[0141]

[0142] As shown in Table 3, the 10 aroma components have a good linear relationship within a certain mass concentration range, and the correlation coefficient (R 2 ) were all greater than 0.9991, and the detection limit (LOD) of the method was 0.050-0.078 mg / L and the quantification limit (LOQ) was 0.166-0.261 mg / L, respectively, calculated by 3 times signal-to-noise ratio (S / N=3) and 10 times signal-to-noise ratio (S / N=10).

[0143] 3. Method accuracy and precision

[0144] Considering that dichloromethane is insoluble in water, and the matrix of rose water is water sample, the mixed standard solution with dichloromethane as solvent was added to the rose water sample. The accuracy of the addition recovery test results needs to be confirmed. In order to make the addition recovery test more accurate and reliable, the test used the standard mixed stock solution with anhydrous ethanol as solvent for the addition recovery test. The standard mixed stock solution III of 10 aroma components at 3 concentration levels was added to ultrapure water, and each concentration level was measured 6 times in parallel to conduct accuracy and precision tests. The results are shown in Table 4.

[0145] Table 4 Accuracy and precision of 10 aroma components

[0146]

[0147]

[0148] As shown in Table 4, the recoveries of the 10 aroma components were 79.806% to 113.780%, and the relative standard deviations (RSDs) were 2.016% to 9.576%. The accuracy and precision of the method met the detection requirements.

[0149] 4. Actual sample analysis

[0150] After the characteristic components of rose water aroma were separated by GC / MS according to the scheme of Example 10, the total ion current diagram of the obtained rose water aroma components is shown in Fig.10 , where a is the total ion current diagram of rose fresh flower cell sap (split ratio 50:1), b is the total ion current diagram of rose water (split ratio 50:1), c is the total ion current diagram of rose fresh flower water (split ratio 50:1), and d is the total ion current diagram of rose salted flower water (split ratio 50:1).

[0151] The method of Example 10 was adopted to respectively measure 10 characteristic aroma components in rose fresh flower cell sap, rose water, rose fresh flower water and rose salted flower water samples, and the contents of rose fresh flower cell sap, rose water, rose fresh flower water and rose salted flower water samples were measured according to the standard curve of Table 3. The results obtained are shown in Table 5.

[0152] Table 5 Actual sample measurement results

[0153]

[0154] As shown in Table 5, the contents of citronellol (120.726 mg / L), nerol (10.176 mg / L), geraniol (47.775 mg / L), benzyl alcohol (94.809 mg / L), phenylethanol (20.499 mg / L), and eugenol (8.817 mg / L) in rose flower cell fluid are significantly higher than those in rose water, rose flower water, and rose salt-preserved flower water samples; the contents of citronellol (50.177 mg / L) and phenylethanol (7.691 mg / L) in rose salt-preserved flower water are significantly higher than those in rose flower water, and the content of linalool (9.242 mg / L) in rose flower water is much higher than that in rose salt-preserved flower water (3.343 mg / L). This method is used to determine 10 aroma components in rose water and rose dew, which is simple to operate, uses less organic solvent, and is suitable for high-throughput analysis of large quantities of samples.

[0155] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for detecting the aroma components of rose water, characterized in that: The following steps are involved: Mixing rose water and a dispersive microextraction solution, and extracting under ultrasonic conditions to obtain an extract; the dispersive microextraction solution is a mixture of an extractant and a dispersant; The extract is subjected to gas chromatography-mass spectrometry detection, and the obtained GC-MS spectrum is searched by using the NIST 11 standard spectrum library to qualitatively identify the aroma components, thereby obtaining the aroma components of rose water; The gas chromatography conditions in the gas chromatography-mass spectrometry detection include: chromatographic column: HP-INNOWAX; programmed temperature: initial temperature 60°C, maintained for 1 min, increased to 245°C / min at a rate of 2°C / min, maintained for 5 min; carrier gas: high-purity helium; injection port temperature: 250°C; non-split injection; The mass spectrometry conditions in the gas chromatography-mass spectrometry detection include: electron bombardment ion source; electron energy: 70eV; mass spectrometry voltage: 0.4kv; transmission line temperature: 250°C; ion source temperature: 230°C; scanning mode: scan mode; mass scanning range: m / z35~500; The rose water aroma components include 2-heptanone, n-dodecane, isopentanol, 2,6,11-trimethyldodecane, 3-methyl-1,5-pentanediol, 2-ethyl-2-hexenal, cyclohexanone, 2-heptanol, methyl heptenone, n-hexanol, rose oxide A, rose oxide B, leaf alcohol, tetradecane, benzyl methyl ether, (S)-linalool oxide, n-heptanol, 6-methyl-5-heptene-2-ol, (E)-linalool oxide, benzaldehyde, linalool, dihydrocarveol, n-heneicosane , 4-terpene alcohol, myrcenol, (-)-trans-pine carveol, furfuryl alcohol, L-menthol, (Z)-3,7-dimethyl-2,6-octadienal, 2-(4-methyl-3-cyclohexenyl)propanal, α-terpineol, verbenol, benzyl acetate, citral, 3,7-dimethyl-7-octenol, citronellol, lavandulol, (-)-myrtenol, nerol, isogeraniol, caryophyllene oxide, phenylethyl acetate, verbenol, geraniol, guaiacol , benzyl alcohol, ocimene, isopulegol, phenylethyl alcohol, 3-(2,6,6-trimethyl-1-cyclohexen-1-yl) acrolein, 2,6-dimethyloct-7-ene-2,6-diol, perillyl alcohol, methyl eugenol, heptanoic acid, 4-tert-butylpropiophenone, 3-phenylpropanol, 4,8-dimethyl-3,7-nonadien-2-yl acetate, p-menthane-1,8-diol, 2,7-dimethyl-2,7-octanediol, 1-cyclohexyl-1-butanone, eucalyptol, Bisabolol oxide B, eugenol, hydroxycitronellol, elemenol, dec-7-en-2-one, isopulegol, cinnamyl alcohol, 2,4-di-tert-butylphenol, (R)-(+)-citronellal acid, farnesol, farnesic acid, neryl acetate, (2E)-3,7-dimethyl-2,6-octadienoic acid, 4-(2,2,6-trimethylcyclohexyl)-2-butanone, 3-ethoxy-3,7-dimethylocta-1,6-diene, elemenol, ceprene, bisabolol, and benzoic acid; The volume ratio of the rose water to the dispersed microextraction solution is 7.0 mL:600 μL; The volume ratio of the extractant to the dispersant is 1:2; The extraction time is 3 min; The extractant is dichloromethane; The dispersant is acetonitrile.

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