Detection method for rapidly detecting 14 sweeteners in Baijiu based on ultra-high performance liquid chromatography tandem mass spectrometer

Abstract

The invention discloses a detection method for rapidly detecting 14 sweeteners in white spirit based on an ultra-high performance liquid chromatography tandem mass spectrometer. The detection method comprises the following steps: S1, preparing reagents and instruments; s2, preparing a standard solution; s3, sample pretreatment; s4, sample detection; s5, establishing a correction curve; and S6, calculating a result. The detection method disclosed by the invention has the characteristics of simplicity, rapidness and good separation effect, plays a positive role in improving the detection efficiency and reducing the detection cost, can meet the requirement of white spirit production enterprises for carrying out daily sweetening agent monitoring work on a large number of samples, and provides technical reference for sweetening agent detection in the field of white spirit circulation.

Description

Technical Field

[0001] The present invention relates to the technical field of liquor brewing, and in particular to a method for rapidly detecting 14 sweeteners in liquor based on ultra-high performance liquid chromatography-tandem mass spectrometry. Background Art

[0002] The brewing process of baijiu (white liquor) is one of my country's invaluable intangible cultural heritage. High-quality baijiu boasts characteristics such as sweetness, richness, and a mellow flavor. This is closely related to the production of higher alcohols and polyols during the natural fermentation process. Sweeteners that may be added to baijiu include both natural and artificial sweeteners. Natural sweeteners include sugars (sucrose and glucose), while others may be synthetic, such as sodium saccharin, sodium cyclamate, acesulfame potassium, and aspartame. Sweeteners are common food additives that can impart sweetness to foods, increase their sweetness, improve their flavor, stimulate appetite, and enhance their quality. As such, while sweeteners, as food additives, can enhance flavor when added in moderation, long-term and excessive intake of artificial sweeteners can lead to metabolic disorders such as hyperglycemia, glucose intolerance, and obesity.

[0003] Sweeteners can be divided into nutritive and non-nutritive sweeteners based on their nutritional value; low-intensity sweeteners and high-intensity sweeteners based on their sweetness; and natural and synthetic sweeteners based on their source. my country's national food safety standard, "Distilled Spirits and Blended Spirits," GB2757-2012, clearly defines distilled spirits as alcoholic beverages made from grains, potatoes, fruits, and dairy products through fermentation, distillation, and blending. However, some unscrupulous manufacturers in the market still deliberately add uncommon artificial sweeteners to their products to sweeten the bitterness of baijiu. This seriously interferes with the healthy development of the baijiu industry and creates unfair competition for genuine baijiu. Therefore, the detection of sweeteners in baijiu is of great significance.

[0004] Currently, the main methods for detecting sweeteners in liquor include high-performance liquid chromatography, ion chromatography, high-performance liquid chromatography-mass spectrometry, ultra-performance liquid chromatography-mass spectrometry, gas chromatography, thin-layer chromatography, and colorimetry. Thin-layer chromatography and colorimetry are primarily used for the detection of cyclamate in food. However, due to their high detection limits, cumbersome procedures, and poor reproducibility, they are rarely used for the detection of sweeteners in food. Furthermore, these two methods have been removed from the revised national standard for the detection of cyclamate in food.

[0005] Since the liquor matrix is ​​complex and contains a large amount of ethanol and other organic components, it may interfere with the detection. The sample pretreatment steps may be cumbersome, such as the need for distillation, extraction and purification processes, which will affect the recovery rate and accuracy. Due to the large differences in the physical and chemical properties of different sweeteners, different detection methods may be required, resulting in low detection efficiency. Although the existing technologies are diverse, they face problems such as matrix interference, complex pretreatment, difficulty in simultaneous detection of multiple components, and standard lag. Therefore, it is very necessary to have a more efficient, sensitive and low-cost detection method. Summary of the Invention

[0006] The technical problem to be solved by the present invention is to address the problems existing in the background technology, thereby providing a detection method based on ultra-high performance liquid chromatography-tandem mass spectrometry. Using this detection method, not only can the detection needs of multiple sweeteners be met at the same time, but it also has the advantages of being fast, simple, and highly sensitive, thereby reducing the detection cost, thereby providing a technical reference for sweetener detection in the field of liquor circulation. Specifically, it is a detection method based on ultra-high performance liquid chromatography-tandem mass spectrometry for rapidly detecting 14 sweeteners in liquor.

[0007] To solve the above technical problems, the technical solution adopted by the present invention is: a detection method for rapidly detecting 14 sweeteners in liquor based on ultra-high performance liquid chromatography tandem mass spectrometry, the detection method comprising the following steps:

[0008] S1. Preparation of reagents and instruments:

[0009] The reagents include 14 sweetener standard substances; chromatographically pure acetonitrile; chromatographically pure acetic acid; distilled water and a microporous filter membrane; and the instrument is a triple quadrupole tandem ultra-high performance liquid chromatograph;

[0010] S2. Standard solution configuration:

[0011] Accurately weigh 25.0 mg of each sweetener standard substance into a 25 mL volumetric flask, dissolve it with distilled water and dilute to the mark to prepare a single standard stock solution with a mass concentration of 1.00 mg / mL, and store it at 0°C for later use; then, respectively pipette 1.00 mL of each single standard stock solution into a 100 mL volumetric flask, dilute it with distilled water and dilute to the mark to prepare a standard intermediate solution. During the test process, use the stepwise dilution method to dilute to the set concentration according to actual needs to prepare standard working solutions of different concentrations, and store them at 4°C in the dark for later use;

[0012] S3. Sample pretreatment:

[0013] Accurately weigh 2.5 g of the liquor to be tested into a 25 mL volumetric flask, dilute to 10.0 mL with distilled water, mix well, filter through a 0.22 μm filter membrane, and then transfer to a sample injection bottle to obtain the sample to be tested;

[0014] S4. Sample testing:

[0015] Using a triple quadrupole tandem ultra-high performance liquid chromatography (UPLC) instrument, 14 sweeteners in the sample were simultaneously determined according to the set detection parameters.

[0016] S5. Establishment of calibration curve:

[0017] The response signal and the concentration of the standard substance are used to establish a calibration curve by taking the logarithm. The model is Y=X a e b , where X is the logarithm of the concentration of the target substance, Y is the logarithm of the corresponding target substance response peak area, and a and b are logarithmic correlation coefficients;

[0018] S6. Calculation results:

[0019] The sample chromatogram is integrated using the established calibration curve, and the calculation formula is:

[0020] Where:

[0021] C is the integrated concentration of the measured component, mg / mL; V is the constant volume, mL; m is the sample amount, g; M is the content of the measured component in the sample, mg / kg.

[0022] Furthermore, the detection method described in the present invention is adopted, wherein, in the sample detection process of step S4, the liquid chromatography conditions adopted are: mobile phase: phase A: 0.2% acetic acid aqueous solution, phase B: methanol; chromatographic column: EClipsePlusC18 chromatographic column 100mm×3.1mm, 1.8m; flow rate: 0.3mL / min; column temperature: 40℃; elution mode is gradient elution.

[0023] Furthermore, the detection method described in the present invention is adopted, wherein, in the sample detection process of step S4, gradient elution is adopted, wherein, when the mobile phase B is gradient eluted, the volume is 0-20%, maintained for 1.5 minutes, within 1.5-3.0 minutes, the volume of mobile phase B is increased from 7% to 50%, and maintained for 2 minutes, to 5.0 minutes, within 5.0-8.0 minutes, the volume of mobile phase B is reduced from 50% to 7%, and maintained for 10 minutes, injection volume: 5 μL, analysis time: 5 minutes.

[0024] Furthermore, the detection method described in the present invention is adopted, wherein, in the sample detection process of step S4, the mass spectrometry conditions adopted are: ion source: electrospray ion source (ESI); scanning mode: negative ion mode scanning; acquisition mode: multiple reaction monitoring (MRM); capillary voltage: 5500V; drying gas temperature: 300℃; drying gas flow rate: 11L / min; sheath gas temperature: 300℃; sheath gas flow rate: 11L / min.

[0025] Furthermore, the detection method of the present invention is used, wherein the 14 sweeteners are acesulfame potassium, cyclamate, saccharin sodium, aspartame, alitame, neotame, sucralose, neohesperidin dihydrochalcone, steviol bioside, steviol bioside, dulcoside A, steviol glycoside, glycyrrhizic acid, rebaudioside A and mogroside V.

[0026] The method for rapidly detecting 14 sweeteners in liquor based on ultra-high performance liquid chromatography-tandem mass spectrometry described in the present invention has the following beneficial effects compared with the prior art: the liquor sample is diluted with distilled water and then passed through a 0.22 μm water filter membrane for direct detection on the machine, and the analysis and detection can be completed within 10 minutes. At two different spike levels, the recovery rate is between 90.54% and 109.73%, and the relative standard deviation (RSD) ranges from 0.51% to 7.32% (n=3). At the same time, by inspecting different brands of liquor on sale, the test results show that the method has the advantages of simple sample pretreatment, low cost, high sensitivity, fast analysis speed and accurate detection results. The recovery rate and reproducibility of the detection method can meet the requirements for qualitative and quantitative analysis of multiple sweeteners in liquor.

[0027] It can be seen that the detection method described in the present invention is simple, fast, and has good separation effect, which plays a positive role in improving detection efficiency and reducing detection costs. It can meet the needs of liquor production companies to carry out daily sweetener monitoring work on a large number of samples, and provides a technical reference for sweetener detection in the liquor circulation field. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The present invention will be described in further detail below with reference to the accompanying drawings.

[0029] Figure 1 This is a TIC diagram of the mass spectrometry signal when formic acid water-methanol is used as the mobile phase for detection;

[0030] Figure 2 This is a TIC diagram of the mass spectrometry signal when ammonium formate-water is used as the mobile phase for detection;

[0031] Figure 3 This is a TIC diagram of the mass spectrometry signal when ammonium acetate-water is used as the mobile phase for detection;

[0032] Figure 4 This is a TIC diagram of the mass spectrometry signal when acetic acid water-methanol is used as the mobile phase for detection;

[0033] Figure 5-6 This is the chromatogram of alitame;

[0034] Figure 7-8 It is the chromatogram of acesulfame potassium;

[0035] Figure 9-10 It is the aspartame chromatogram;

[0036] Figure 11-12 is the chromatogram of dulcoside A;

[0037] Figure 13-14 is the chromatogram of glycyrrhizic acid;

[0038] Figure 15-16 is the chromatogram of mogroside V;

[0039] Figure 17-18 This is the chromatogram of neotame;

[0040] Figure 19-20 is the chromatogram of rebaudioside A;

[0041] Figure 21-22 is the chromatogram of sucralose;

[0042] Figure 23-24 It is the chromatogram of sodium saccharin;

[0043] Figures 25-26 This is the chromatogram of steviol bioside;

[0044] Figure 27 It is a chromatogram of cyclamate;

[0045] Figures 28-29 This is the chromatogram of neohesperidin dihydrochalcone;

[0046] Figure 30 This is a chromatogram of steviol glycosides. DETAILED DESCRIPTION

[0047] The following describes the implementation of the present invention through specific embodiments. People skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification.

[0048] It should be noted that the term "comprise" or any other variation is intended to cover non-exclusive inclusion, so that a process, method, article or apparatus that includes a series of elements includes not only those elements, but also includes other elements not explicitly listed, or also includes elements that are inherent to such process, method, article or apparatus.

[0049] The technical solution of the present invention is further analyzed and explained below through specific embodiments.

[0050] The present invention provides a method for rapidly detecting 14 sweeteners in liquor based on ultra-high performance liquid chromatography-tandem mass spectrometry, the method comprising the following steps:

[0051] 1. Materials and Reagents

[0052] Acetonitrile (chromatographically pure) was produced by Tianjin Comeo Chemical Reagent Co., Ltd.; acetic acid (chromatographically pure) was produced by Tianjin Comeo Chemical Reagent Co., Ltd.; 14 kinds of sweetener standard substances were: acesulfame potassium, cyclamate, saccharin sodium, aspartame, alitame, neotame, sucralose, neohesperidin dihydrochalcone, stevioside, dulcoside A, steviol glycosides, glycyrrhizic acid, rebaudioside A, and mogroside V standard substances, with a purity of ≥97%, and were produced by Tanmo Quality Inspection Technology Co., Ltd.; distilled water was produced by Watsons, and the microporous filter membrane was 0.22m (aqueous phase). The liquor samples used in this experiment were all commercially purchased.

[0053] 2. Standard solution preparation

[0054] Accurately weigh 25.0 mg of each sweetener into a 25 mL volumetric flask, dissolve and dilute to volume with distilled water to prepare 14 single-standard stock solutions of sweeteners with a mass concentration of 1.00 mg / mL, and store or preserve at 0°C. In the specific testing stage, respectively, draw 1.00 mL of each single-standard stock solution into a 100 mL volumetric flask, dilute and dilute to volume with distilled water to prepare standard intermediate solutions of 14 sweeteners. During the specific test process, use the stepwise dilution method to dilute to the appropriate concentration according to actual needs in order to prepare standard working solutions of different concentrations, and store at 4°C in the dark for future use.

[0055] 3. Sample pretreatment

[0056] Accurately weigh 2.5 g (accurate to 0.01 g) of the liquor to be tested and place it in a 25 mL volumetric flask. After passing through a 0.22 μm filter membrane, transfer it to an injection bottle for liquid chromatography-tandem mass spectrometry determination.

[0057] 4. Establishment of calibration curve

[0058] Calibration curve establishment: Use the response signal and the standard substance concentration to take the logarithm to establish the calibration curve model Y = X a e b , where X is the logarithm of the target substance concentration, Y is the logarithm of the corresponding target substance response peak area, and a and b are logarithmic correlation coefficients.

[0059] 5. Sample testing

[0060] Using ultra-high performance liquid chromatography (UPLC) and triple quadrupole tandem mass spectrometry (MS / MS), 14 sweeteners in the sample were simultaneously determined according to the set detection parameters.

[0061] 6. Calculation results

[0062] The sample chromatogram is integrated using the established calibration curve, and the calculation formula is:

[0063] Where:

[0064] C is the integrated concentration of the measured component, mg / mL; V is the constant volume, mL; m is the sample amount, g; M is the content of the measured component in the sample, mg / kg.

[0065] The detection method of the present invention is used, in the specific detection process, the instruments and equipment used are a triple quadrupole tandem ultra-high performance liquid chromatograph, model 1290Ⅱ-6460C (equipped with an electrospray ion source), a product produced by Agilent Technologies, USA; at the same time, a 1 / 10,000 analytical balance is required, which is a product produced by Mettler-Toledo.

[0066] Among them, during the sample detection process, the liquid chromatography conditions are:

[0067] Mobile phase: Phase A: 0.2% acetic acid in water, Phase B: methanol; Column: EClipse Plus C18 column, 100 mm × 3.1 mm, 1.8 μm; Flow rate: 0.3 mL / min; Column temperature: 40°C; Injection volume: 5 μL. Elution: Gradient elution: Phase B 20% (hold) for 1.5 min, then 7% to 50% (hold) for 2 min from 1.5 to 3.0 min, then 50% to 7% (hold) for 10 min from 5.0 to 8.0 min. Injection volume: 5 μL; Analysis time: 5 min. Specific LC conditions are shown in Table 1.

[0068] Table 1 Liquid chromatography conditions

[0069] Time / min Mobile phase A% Mobile phase B% 0 93 7 1.5 93 7 3.0 50 50 5.0 50 50 8.0 93 7 10.0 93 7

[0070] During the sample detection process, the mass spectrometry conditions are:

[0071] Ion source: electrospray ionization (ESI); Scan mode: negative ion mode; Acquisition mode: multiple reaction monitoring (MRM); Capillary voltage: 5500 V; Drying gas temperature: 300°C; Drying gas flow rate: 11 L / min; Sheath gas temperature: 300°C; Sheath gas flow rate: 11 L / min. Specific mass spectrometry analysis parameters for the 14 sweeteners are shown in Table 2.

[0072] Table 2 Mass spectrometry analysis parameters of 14 sweeteners

[0073]

[0074] Using the detection method provided by the present invention, through the study of the physicochemical properties of 14 sweeteners, it was established that a C18 chromatographic column was used to separate the target compounds. The specific liquid chromatography conditions were selected and optimized as follows:

[0075] 14 compound standard solutions were analyzed by injection using 0.2% formic acid water-methanol, 10mmol ammonium formate-water, 10mmol ammonium acetate-water, and 0.2% acetic acid water-methanol as the mobile phases. The experimental results show that when 0.2% acetic acid water-methanol is used as the mobile phase, the compound signal response intensity is the highest; and when 0.2% acetic acid water-methanol is used as the mobile phase, the peak time of each substance is the earliest and the reaction time is the shortest. According to the liquid chromatography conditions in Table 1, when gradient elution is used, the separation effect of each compound is good and the mass spectrometry signal response is strong. The TIC diagrams of the mass spectrometry signals under the four mobile phases are as follows: Figures 1 to 4 As shown, when 0.2% acetic acid water-methanol is used as the mobile phase, the chromatograms of the 14 sweeteners, namely the MRM diagrams, are as follows: Figures 5 to 30 Therefore, this scheme finally selected 0.2% acetic acid water-methanol as the mobile phase for gradient elution.

[0076] Using the detection method provided by the present invention, in the actual sample measurement process, according to the above detection method, the content of 14 sweeteners in 9 currently available commercial liquor samples (specific liquor brand names are not specified) was detected. Each sample was measured three times. The results showed that none of the 14 sweeteners were detected in the 9 liquor samples. The specific sample detection results are shown in Table 3.

[0077] Table 3 Sample test results

[0078] name ZJ-1 ZJ-2 XJ-1 XJ-2 XJ-3 MT-1 MT-1 JS-1 DYT-1 Acesulfame K ND ND ND ND ND ND ND ND ND cyclamate ND ND ND ND ND ND ND ND ND Saccharin sodium ND ND ND ND ND ND ND ND ND Aspartame ND ND ND ND ND ND ND ND ND Alitame ND ND ND ND ND ND ND ND ND Neotame ND ND ND ND ND ND ND ND ND Sucralose ND ND ND ND ND ND ND ND ND Neohesperidin dihydrochalcone ND ND ND ND ND ND ND ND ND Stevioside ND ND ND ND ND ND ND ND ND Dulcoside A ND ND ND ND ND ND ND ND ND Stevioside ND ND ND ND ND ND ND ND ND Glycyrrhizic acid ND ND ND ND ND ND ND ND ND Rebaudioside A ND ND ND ND ND ND ND ND ND Mogroside V ND ND ND ND ND ND ND ND ND

[0079] Note: ND means not detected.

[0080] In order to illustrate the advantages of the detection method provided by the present invention, the linear range and the detection limit and quantification limit of the method are described as follows:

[0081] The target standard stock solutions were diluted with mobile phase to prepare 14 different sweetener standard working solutions. These solutions were analyzed using UPLC-MS / MS under chromatographic-mass spectrometric conditions, and standard working curves were plotted. The limit of detection (LOD) was determined using a signal-to-noise ratio (S / N) of 3, and the limit of quantification (LOQ) was determined using a signal-to-noise ratio (S / N) of 10. The 14 sweeteners showed good linearity within their respective concentration ranges, with correlation coefficients (R) of no less than 0.9991 for each substance, indicating low limits of detection and high sensitivity. The specific detection results for the 14 sweeteners in liquor are shown in Table 4.

[0082] Table 4 Linear equations, correlation coefficients, linear ranges and detection limits of 14 sweeteners in liquor

[0083]

[0084] From the results in Table 4, it can be seen that the linear relationships of the 14 sweeteners are all between 0.991 and 0.9999.

[0085] In addition, in order to illustrate the advantages of the detection method provided by the present invention, the precision and recovery are described:

[0086] The recovery rate test of liquor samples was carried out by adding standard solution to blank samples. The three concentration levels of spiked liquor were 500 μg / L and 1000 μg / L, and the experiment was repeated three times for each concentration level. The recoveries and relative standard deviations of 14 sweeteners in liquor are shown in Table 5.

[0087] Table 5 Recovery rates and relative standard deviations of 14 sweeteners spiked in liquor

[0088]

[0089]

[0090] The results in Table 5 show that the recoveries of the 14 sweeteners ranged from 90% to 109%, with relative standard deviations less than 8%. This indicates that the recovery and relative standard deviations of this method meet the requirements of relevant domestic and international standards and regulations and can be used for the simultaneous detection of 14 sweeteners in liquor.

[0091] Thus, using the detection method provided by the present invention, liquor samples can be directly analyzed within 10 minutes after being diluted with distilled water and filtered through a 0.22μm water filter membrane. Furthermore, at two different spike levels, the recovery rate ranged from 90.54% to 109.73%, and the relative standard deviation (RSD) ranged from 0.51% to 7.32% (n=3). Furthermore, different brands of liquor were tested. The results demonstrated that this method offers advantages such as simple sample pretreatment, low cost, high sensitivity, rapid analysis, and accurate test results. The method's recovery rate and reproducibility meet the requirements for qualitative and quantitative analysis of various sweeteners in liquor, making it suitable for liquor manufacturers to conduct routine sweetener monitoring on large numbers of samples. This provides a technical reference for sweetener detection in the liquor distribution industry.

[0092] Other aspects of the present invention that are not described in detail are all conventional techniques known to those skilled in the art.

[0093] The protection scope of the present invention is not limited to the technical solutions disclosed in the specific implementation methods. The above description is only a preferred implementation method of the present invention and does not limit the present invention. Any minor modifications, equivalent replacements and improvements made based on the technical solutions of the present invention should be included in the protection scope of the technical solutions of the present invention.

Claims

1. A method for rapid detection of 14 sweeteners in liquor based on ultra-high performance liquid chromatography-tandem mass spectrometry, characterized in that: The detection method comprises the following steps: S1. Preparation of reagents and instruments: The reagents include 14 sweetener standard substances; chromatographically pure acetonitrile; chromatographically pure acetic acid; distilled water and a microporous filter membrane; and the instrument is a triple quadrupole tandem ultra-high performance liquid chromatograph; S2. Standard solution configuration: Accurately weigh 25.0 mg of each of the 14 sweetener standard substances into a 25 mL volumetric flask, dissolve them in distilled water and dilute to the mark to prepare a single standard stock solution with a mass concentration of 1.00 mg / mL. Store at 0°C until use. Then, pipette 1.00 mL of each single standard stock solution into a 100 mL volumetric flask, dilute it with distilled water and make up to the mark to prepare the standard intermediate solution. During the test process, use the stepwise dilution method to dilute it to the set concentration according to actual needs to prepare standard working solutions of different concentrations. Store it in the dark at 4°C until use. S3. Sample pretreatment: Accurately weigh 2.5 g of the liquor to be tested into a 25 mL volumetric flask, dilute to 10.0 mL with distilled water, mix well, filter through a 0.22 μm filter membrane, and then transfer to a sample injection bottle to obtain the sample to be tested; S4. Sample testing: Using a triple quadrupole tandem ultra-high performance liquid chromatography (UPLC) instrument, 14 sweeteners in the sample were simultaneously determined according to the set detection parameters. S5. Establishment of calibration curve: The response signal and the concentration of the standard substance are used to establish a calibration curve by taking the logarithm. The model is Y=X a e b , where X is the logarithm of the concentration of the target substance, Y is the logarithm of the corresponding target substance response peak area, and a and b are logarithmic correlation coefficients; S6. Calculation results: The sample chromatogram is integrated using the established calibration curve, and the calculation formula is: C is the integrated concentration of the measured component, mg / mL; V is the constant volume, mL; m is the sample amount, g; M is the content of the measured component in the sample, mg / kg.

2. The detection method according to claim 1, wherein: During the sample detection process in step (4), the liquid chromatography conditions used are as follows: mobile phase: phase A: 0.2% acetic acid aqueous solution, phase B: methanol; chromatographic column: EClipse Plus C18 chromatographic column 100 mm × 3.1 mm, 1.8 m; flow rate: 0.3 mL / min; column temperature: 40°C; and elution mode is gradient elution.

3. The detection method according to claim 1, wherein: During the sample detection process in step (4), gradient elution is performed by elution mode, wherein, when gradient elution is performed, the volume of mobile phase B is 0-20% and maintained for 1.5 min. Within 1.5-3.0 min, the volume of mobile phase B is increased from 7% to 50% and maintained for 2 min to 5.0 min. Within 5.0-8.0 min, the volume of mobile phase B is reduced from 50% to 7% and maintained for 10 min. The injection volume is 5 μL and the analysis time is 5 min.

4. The detection method according to claim 1, wherein: During the sample detection process in step (4), the mass spectrometry conditions used are: ion source: electrospray ion source (ESI); scanning mode: negative ion mode scanning; acquisition mode: multiple reaction monitoring (MRM); capillary voltage: 5500 V; drying gas temperature: 300°C; drying gas flow rate: 11 L / min; sheath gas temperature: 300°C; sheath gas flow rate: 11 L / min.

5. The detection method according to claim 1, wherein: The 14 sweeteners are acesulfame potassium, cyclamate, saccharin sodium, aspartame, alitame, neotame, sucralose, neohesperidin dihydrochalcone, steviol bioside, dulcoside A, steviol glycoside, glycyrrhizic acid, rebaudioside A, and mogroside V.

Images