A method for simultaneously determining contents of various components in Yinhu Ganmao Powder based on GC-MS technology

Abstract

The present application relates to the field of pharmaceutical analysis, and more particularly to a method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder based on GC-MS technology, which comprises a method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder or volatile oil. The method comprises the following steps: (1) performing GC analysis on the extract of Yinhu Ganmao Powder or volatile oil; (2) performing mass spectrometry identification using a mass spectrometry library, with the mass spectrometry conditions being: ion source is electron impact ionization (EI), energy is 70 eV, ion source temperature is 200 DEG C, interface temperature is 250 DEG C, full scan mode is m / z 45-500, electron multiplier voltage is 1.5 kV, and collision gas is argon (99.99%). The present application establishes a method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder or volatile oil based on GC-MS technology, wherein more than 50 compounds are identified in the volatile oil of Yinhu Ganmao Powder, and more than 25 compounds are identified in the n-hexane extract of the powder.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of pharmaceutical analysis, in particular to a method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder based on GC-MS technology. BACKGROUND

[0002] Yinhu Ganmao Powder is composed of 12 medicinal materials, such as Pinus densata, Eucalyptus globulus, Lonicera japonica, Forsythia suspensa, Schizonepeta, Bupleurum, Artemisia annua, Mentha haplocalyx, Pogostemonis Herba, Citrus reticulata, Platycodon grandiflorum, and Artemisia argyi, and has the functions of dispelling wind and relieving superficies and clearing heat and resolving toxicity. It is usually used for treating aversion to cold and fever, nasal obstruction and sneezing, cough, headache, and general malaise caused by wind-heat cold. It plays a great role in the treatment of pneumonia caused by the new coronavirus. The volatile oil of Yinhu Ganmao Powder is composed of medicinal powder and medicinal oil. During the preparation process, the volatile oil is extracted from each medicinal material by steam distillation, and the volatile oil is mixed to become medicinal oil. After the extraction of volatile oil from Lonicera japonica, Forsythia suspensa, and other medicinal materials, the remaining medicinal residues are crushed and dried to form medicinal powder. Before use, the medicinal oil of Yinhu Ganmao Powder volatile oil is poured into the medicinal powder and applied to the navel for transdermal absorption into the human body to produce a therapeutic effect. The effective material basis of the volatile oil of Yinhu Ganmao Powder comes from multiple active ingredients in multiple medicinal ingredients. The current quality standard of the volatile oil of Yinhu Ganmao Powder only determines the content of chlorogenic acid, and lacks a method for effectively evaluating the overall quality of the volatile oil of Yinhu Ganmao Powder. Therefore, it is necessary to establish a comprehensive evaluation method for the quantitative determination of multiple components in the volatile oil of Yinhu Ganmao Powder.

[0003] Currently, there is no report on a method for simultaneously determining the contents of multiple components in the medicinal powder or volatile oil of Yinhu Ganmao Powder based on GC-MS technology. SUMMARY

[0004] In order to overcome the deficiencies of the prior art, the present application provides a method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder based on GC-MS technology.

[0005] The object of the present application can be achieved by the following technical solutions:

[0006] A method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder based on GC-MS technology, which comprises a method for simultaneously determining the contents of multiple components in the medicinal powder or volatile oil of Yinhu Ganmao Powder, comprising the following steps:

[0007] (1) performing GC analysis program on the extract of Yinhu Ganmao Powder medicinal powder or volatile oil;

[0008] (2) Mass spectrometry identification by mass spectrometry library, mass spectrometry conditions: ion source is electron impact ionization (EI), energy is 70 eV, ion source temperature is 200℃, interface temperature is 250℃, full scan mode m / z 45-500, electron multiplier voltage is 1.5 kV, collision gas is argon (99.99%).

[0009] Preferably, the mass spectrometry library comprises one of NIST20-1, NIST20-2, NIST20s or a combination of two or more thereof.

[0010] Preferably, the GC analysis procedure of the volatile oil of the Yinhugan'ganmaosan is as follows: column temperature is 80℃ for 10 min, increased to 150℃ at a rate of 10℃ / min for 30 min, increased to 200℃ at a rate of 25℃ / min for 15 min, carrier gas is nitrogen (99.99%), split ratio is 10:1, injection volume is 1 μL, injection port temperature is 200℃, and detector temperature is 250℃.

[0011] Preferably, the Yinhugan'ganmaosan powder extract is a n-hexane extract of the Yinhugan'ganmaosan powder, and the GC analysis procedure of the n-hexane extract of the Yinhugan'ganmaosan powder is as follows: column temperature is 50℃ for 1 min, increased to 180℃ at a rate of 10℃ / min for 30 min, and increased to 240℃ at a rate of 10℃ / min for 30 min, carrier gas is nitrogen (99.99%), split ratio is 10:1, injection volume is 1 μL, injection port temperature is 200℃, and detector temperature is 250℃.

[0012] Preferably, the volatile oil of the Yinhugan'ganmaosan is prepared as follows: Gangsong and Eucalyptus globulus leaves are crushed and soaked in water at a ratio of 1 g:15 ml, followed by steam distillation for 2.5 h, and the volatile oil is collected and stored in another container; Artemisia carvifolia, Schizonepeta, Mentha, Forsythia, Pogostemonis, Artemisia argyi, and Citrus reticulata are crushed and soaked in water at a ratio of 1 g:15 ml, followed by steam distillation for 3 h, and the collected volatile oils are mixed uniformly, and a proper amount of the mixed volatile oil is diluted 20,000 times with N,N-dimethylformamide, and then filtered through a 0.22 μm organic phase filter for GC-MS analysis.

[0013] Preferably, the amount of each medicinal material is as follows: Gangsong 6818 g, Eucalyptus globulus leaves 6818 g, Artemisia carvifolia 45 g, Schizonepeta 45 g, Mentha 45 g, Forsythia 45 g, Pogostemonis 45 g, Artemisia argyi 23 g, and Citrus reticulata 23 g.

[0014] Preferably, the n-hexane extract of the Yinhugan'ganmaosan powder is prepared as follows: 1.0 g of the powder in the Yinhugan'ganmaosan is weighed into a conical flask, 10 ml of n-hexane is added, and the mixture is ultrasonically extracted for 30 min, cooled, weighed, centrifuged at 8000 rpm for 20 min, and the supernatant is filtered through a 0.22 μm filter for GC-MS analysis.

[0015] The application also provides a method for simultaneously determining the contents of multiple components in volatile oil of Yinhu Ganmao Powder based on GC-MS technology combined with MRM, and the mass evaluation method comprises the following steps:

[0016] (1) Preparation of volatile oil of Yinhu Ganmao Powder: take Gongsong 6818 g and Daye Eucalyptus leaf 6818 g, crush them, and then soak them in water at 1 g:15 ml, and then perform water vapor distillation for 2.5 h, collect the volatile oil, and store it in another container; take Artemisia argyi, Schizonepeta, Mentha, Forsythia, Pogostemonis Herba, and Folium Bupleuri each 45 g, and take Pericarpium Citri Reticulatae and Folium Artemisiae Argyi each 23 g, crush them, and then soak them in water at 1 g:15 ml, and then perform water vapor distillation for 3 h, collect the volatile oil, and mix the collected volatile oils evenly, take a proper amount of the mixed volatile oil, dilute it with N,N-dimethylformamide at 20000 times, and then perform GC-MS analysis after passing through a 0.22 μm organic phase filter membrane;

[0017] (2) The GC analysis procedure of the volatile oil of Yinhu Ganmao Powder is as follows: the column temperature is kept at 80 ℃ for 10 min, is increased to 150 ℃ at a speed of 10 ℃ / min and is kept at 150 ℃ for 30 min, is increased to 200 ℃ at a speed of 25 ℃ / min and is kept at 200 ℃ for 15 min, the carrier gas is nitrogen (99.99%), the split ratio is 10:1, the injection amount is 1 μL, the injection port temperature is 200 ℃, and the detector temperature is 250 ℃;

[0018] (3) Mass spectrum identification is performed by using a mass spectrum library (NIST20-1, NIST20-2 and NIST20s), and the mass spectrum conditions are as follows: the ion source is electron impact ionization (EI), the energy is 70 eV, the ion source temperature is 200 ℃, the interface temperature is 250 ℃, the full scan mode is m / z 45-500, the electron multiplier voltage is 1.5 kV, and the collision gas is argon (99.99%);

[0019] (4) The mass spectrum identification results are combined with multiple reaction monitoring (MRM) to perform detection analysis and content determination of the components.

[0020] Compared with the prior art, the method of the application has the following advantages:

[0021] 1. The method for simultaneously determining the contents of multiple components in Yinhu Ganmao Powder or volatile oil of Yinhu Ganmao Powder is established by using GC-MS technology, more than 50 compounds are identified in the volatile oil of Yinhu Ganmao Powder, and more than 25 compounds are identified in the n-hexane extract of the powder.

[0022] 2. The method for performing MRM quantitative analysis on 19 compounds in the volatile oil of Yinhu Ganmao Powder is established, the quantitative results of the 19 components in the volatile oil of Yinhu Ganmao Powder are reliable, and the specific contents of the 19 compounds with relatively high contents in the volatile oil of Yinhu Ganmao Powder are further determined. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1GC-MS total ion chromatogram of volatile oil of Yinhu colds powder.

[0024] Figure 2 GC-MS total ion chromatogram of n-hexane extract of Yinhu colds powder.

[0025] Figure 3 GC-MS chromatogram of MRM extraction of 19 components of volatile oil of Yinhu colds powder. (A. α-pinene; B. camphene; C. sabinene; D. β-pinene; E. α-terpinene; F. limonene; G. P-cymene; H. eucalyptol; I. linalool; J. (-)-menthone; K. 4-terpeniol; L. menthol; M. α-terpineol; N. tridecane; O. pulegone; P. trans-caryophyllene; Q. α-caryophyllene; R. hexadecane; S. patchoulil). DETAILED DESCRIPTION

[0026] The following examples are used to illustrate the present application, but are not used to limit the scope of the present application.

[0027] Example 1

[0028] I. Experimental materials

[0029] 1.1 Instruments and equipment

[0030] Nexis TQ2030 type GC (Shimadzu Corporation, Japan); TQ8040 Nexis type MS (Shimadzu Corporation, Japan); DB-624UI gas chromatographic column (30 m x 0.25 mm x 1.40 μm, Agilent Corporation, USA); high-speed low-temperature centrifuge (SIGMA Corporation, Germany); carbon dioxide incubator (Yisigao Medical Technology Co., Ltd., Taicang); microplate reader (TECAN Corporation, Switzerland); analytical balance (Mettler Toledo Technology Co., Ltd.).

[0031] 1.2 Reagents and reagents

[0032] Medicinal materials and reagents Yinhu Ganmao Powder (202106291, 202101233, 2021103082) were provided by Guangxi Yuanantang Pharmaceutical Co., Ltd.; N,N-dimethylformamide (DMF, HPLC≥99.9, C14428283) and dimethyl sulfoxide (DMSO, HPLC≥99.9, C14585519) were purchased from Shanghai MacLin Biochemical Technology Co., Ltd.; a-pinene (98%, CFN70238), β-pinene (98%, CFN93287), a-pinene (98%, CFN93285), trans-caryophyllene (98%, CFN90502), 4-terpenol (98%, CFN94877), a-pinene (98%, CFN70238) were purchased from chemfaces company; tridecane (98.5%, 190191-201701), linalool (98.8%, 111503-202004), menthone (99.8%, 111706-201907), (-)-menthone (99.9%, 111705-202106), menthol (99.8%, 110728-201707), limonene (96%, 100470-201302), dexamethasone sodium phosphate (100016-202117) were purchased from China Institute of Food and Drug Control; a-terpineol (98.7%, 0913-RC-OO42) and camphene (99.4%, D6-12-5-1) were purchased from CATO; eucalyptol (98%, 221212), hexadecane (99.5%, 20230320), P-cymene (98%, 230505) were purchased from Beijing North Great Metrology Technology Research Institute; patchoulol (97%, Shanghai Acemec Biochamical, 95523846C); sylvestrene (98%, Shanghai Yuanye Biological Technology Co., Ltd., M23HB179089); a-caryophyllene (95%, Hebei Bailinwei Superfine Material Co., Ltd., L310X43).

[0033] II. Experimental methods

[0034] 2.1 Preparation of volatile oil of Yinhu Ganmao Powder

[0035] Take Gongsong 6818 g and Eucalyptus globulus 6818 g, crush them, and then soak them in water at 1 g: 15 ml, followed by water vapor distillation for 2.5 h, collect the volatile oil, and store it in another container; Artemisia argyi, Schizonepeta, Mentha, Forsythia, Pogostemonis Herba, each 45 g, and Folium Artemisiae Argyi, Pericarpium Citri Reticulatae, each 23 g, crush them, and then soak them in water at 1 g: 15 ml, followed by water vapor distillation for 3 h, collect the volatile oil, mix the collected volatile oils uniformly, take an appropriate amount of mixed volatile oil, dilute it 20000 times with N,N-dimethylformamide, and then pass it through a 0.22 μm organic phase filter membrane for GC-MS analysis.

[0036] 2.2 Preparation of n-hexane extract of Yinhuganmaosan powder

[0037] 1.0 g of Yinhuganmaosan powder was weighed into a conical flask, 10 ml of n-hexane was added, and the weight was recorded. The mixture was extracted by ultrasonic for 30 min, cooled, and the weight was made up. The mixture was centrifuged at 8000 rpm for 20 min, and the supernatant was filtered through a 0.22 μm filter membrane for GC-MS analysis.

[0038] 2.3 GC-MS conditions

[0039] The GC analysis program for the volatile oil of Yinhuganmaosan was as follows: 80℃ for 10 min, 10℃ / min to 150℃ for 30 min, 25℃ / min to 200℃ for 15 min, nitrogen gas (99.99%) as carrier gas, split ratio of 10:1, sample injection amount of 1 μL, sample injection port temperature of 200℃, and detector temperature of 250℃.

[0040] The GC analysis program for the n-hexane extract of Yinhuganmaosan powder was as follows: 50℃ for 1 min, 10℃ / min to 180℃ for 30 min, 10℃ / min to 240℃ for 30 min, nitrogen gas (99.99%) as carrier gas, split ratio of 10:1, sample injection amount of 1 μL, sample injection port temperature of 200℃, and detector temperature of 250℃.

[0041] Mass spectrometry conditions: ion source was electron impact ionization (EI), energy was 70 eV, ion source temperature was 200℃, interface temperature was 250℃, full scan mode m / z 45-500, electron multiplier voltage was 1.5 kV, and collision gas was argon (99.99%).

[0042] 2.4 Mass spectrometric identification of components of volatile oil and powder

[0043] Compound identification was performed by literature review and NIST20-1, NIST20-2, and NIST20s databases using Shimadzu reanalysis software. We also checked the mass-to-charge ratio and relative abundance conditions of the mass spectrometric data as a visual comparison.

[0044] 2.5 MRM quantitative analysis of target compounds

[0045] After comparing precursor ion data with standard databases NIST20-1, NIST20-2, NIST20s, and literature review, the present study quantitatively analyzed 19 compounds with relatively high content in volatile oil. First, the product ion scan was performed on target compounds to optimize the optimal fragmentation voltage of product ion fragments and determine the Q3 ion of MRM. According to the MRM scan on the mixed standard solution, the ion ratio of MRM method was reset to establish the MRM quantitative analysis method for the 19 compounds.

[0046] III. Experimental results

[0047] 3.1 GC-MS identification results of volatile oil in Yinhu cold powder

[0048] The Q3Scan full scan method was used to analyze the components of volatile oil. Figure 1 The total ion chromatogram (TIC) of volatile oil in Yinhu cold powder was obtained. According to the literature review and database data, as well as the mass-to-charge ratio and relative abundance of base peak, a total of 50 compounds were identified (Table 1), among which the relative content of eucalyptol was the highest, accounting for 28.25%.

[0049] 3.2 GC-MS identification results of n-hexane extract of Yinhu cold powder

[0050] The Q3Scan method was used to analyze the components of n-hexane extract of Yinhu cold powder. Figure 2 According to the literature review and database data, as well as the mass-to-charge ratio and relative abundance of base peak, a total of 25 compounds were identified (Table 2), among which the content of eucalyptol was the highest, accounting for 34.83%. The identification results of the top relative content components were the same as those in volatile oil, so the 50 compounds identified in the volatile oil were used for subsequent network pharmacology analysis.

[0051] 3.3 MRM quantitative analysis of 19 compounds in volatile oil of Yinhu cold powder

[0052] In order to determine the content of the relatively high content components in volatile oil of Yinhu cold powder, 19 components were selected for quantitative analysis according to the relative percentage content and the availability of standard on the market. The positioning results of standard and components in volatile oil are as follows: Figure 3As shown, the retention time of 19 compounds was consistent with the volatile oil, and the solvent DMF had no interference with the detection. The product ion scanning conditions of 19 target compounds were optimized to obtain the optimal CE voltage and ion abundance of each target component. The results are shown in Table 3. According to the optimal CE voltage, the quantitative ion pair and the qualitative ion pair, the MRM method was established, the standard solution was configured, and the methodological verification was performed with N,N-dimethylformamide as the solvent blank. The results showed that the solvent had no interference with the detection, and the MRM extraction mass chromatogram peak of the volatile oil of Yinhuganliao San was consistent with the RT of the standard solution.

[0053] 3.4 Methodological investigation

[0054] The 19 mixed compounds were configured at different concentrations to establish the GC-MS quantitative method for 19 compounds. The results (Table 4) showed that the established method was linear, stable, reproducible, precise and accurate, indicating that the quantitative results of 19 components in the volatile oil of Yinhuganliao San were reliable, and the specific content of the 19 compounds with higher relative content in the volatile oil of Yinhuganliao San was further determined.

[0055] Table 1 GC-MS identification results of volatile oil of Yinhuganliao San

[0056]

[0057]

[0058]

[0059] Table 2 GC-MS identification results of n-hexane extract of Yinhuganliao San powder

[0060]

[0061]

[0062] Table 3 Quantitative and qualitative ion pair information of 19 compounds in volatile oil of Yinhuganliao San

[0063]

[0064]

[0065] Table 4 Content determination of 19 components in Yinhuganliao San

[0066]

[0067]

[0068] While the application has been described in detail and with reference to specific embodiments thereof, it will be apparent to those skilled in the art that various modifications and improvements can be made to the application. Accordingly, no limitation is implied by the description went to the particulars of the application. Rather, the spirit and scope of the application are to be indicated by the appended claims and their equivalents.

Claims

1. A method for simultaneously determining the content of multiple components in Yin Hu Ganmao San (a traditional Chinese medicine formula) based on GC-MS technology, the method comprising simultaneously determining the content of multiple components in Yin Hu Ganmao San powder or volatile oil, characterized in that, The method includes the following steps: (1) Perform GC analysis on the extract or volatile oil of Yin Hu Ganmao San (a traditional Chinese medicine for colds); (2) Mass spectrometry identification using a mass spectrometry library. Mass spectrometry conditions: the ion source is electron bombardment ionization with an energy of 70 eV, the ion source temperature is 200℃, the interface temperature is 250℃, the full scan mode is m / z 45-500, the electron multiplication voltage is 1.5 kV, and the collision gas is argon with a purity of 99.99%. The GC analysis procedure for the volatile oil of Yin Hu Ganmao San was as follows: column temperature 80℃ held for 10 min, increased to 150℃ at a rate of 10℃ / min and held for 30 min, increased to 200℃ at a rate of 25℃ / min and held for 15 min, carrier gas was nitrogen with a purity of 99.99%, split ratio was 10:1, injection volume was 1 μL, injection port temperature was 200℃, and detector temperature was 250℃. Preparation of the volatile oil from Yin Hu Ganmao San: Take Pinus massoniana and Eucalyptus grandis leaves, crush them, soak them in water at a ratio of 1g:15ml, and then steam distill for 2.5 seconds. h, collect the volatile oil and store it separately; Artemisia annua, Schizonepeta tenuifolia, Mentha haplocalyx, Forsythia suspensa, Pogostemon cablin, Artemisia argyi, and Citrus reticulata peel are pulverized and soaked in water at a ratio of 1g:15ml, followed by steam distillation for 3 hours, and the volatile oil is collected. The collected volatile oil is mixed evenly, and an appropriate amount of the mixed volatile oil is diluted 20,000 times with N,N-dimethylformyl and then filtered through a 0.22μm organic phase filter membrane for GC-MS analysis; the compounds contained in the volatile oil of Yin Hu Ganmao San include: α-pinene, camphene, sabinene, β-pinene, α-terpinene, limonene, p-cymene, eucalyptol, linalool, (-)-menthone, 4-terpene alcohol, menthol, α-terpineol, tridecane, menthol, transcaryophyllene, α-caryophyllene, hexadecane, and patchouli alcohol; The extract of Yin Hu Ganmao San (a traditional Chinese medicine) powder is a hexane extract of Yin Hu Ganmao San powder. The GC analysis procedure for the hexane extract of Yin Hu Ganmao San powder is as follows: column temperature 50℃ for 1 min, rising to 180℃ at 10℃ / min and holding for 30 min, rising to 240℃ at 10℃ / min and holding for 30 min, carrier gas is nitrogen with a purity of 99.99%, split ratio is 10:1, injection volume is 1 μL, injection port temperature is 200℃, and detector temperature is 250℃. The compounds contained in the hexane extract of Yin Hu Cold Powder include: α-pinene, camphene, sabinene, β-pinene, α-terpinene, limonene, p-cymene, eucalyptol, linalool, (-)-menthone, 4-terpene alcohol, menthol, α-terpineol, tridecane, menthol, transcaryophyllene, α-caryophyllene, hexadecane, and patchouli alcohol.

2. The method according to claim 1, characterized in that, The mass spectrometry library includes one or more of NIST20-1, NIST20-2, and NIST20s.

3. The method according to claim 2, characterized in that, The ingredients for the various medicinal materials are: 6818g of Pinus massoniana, 6818g of Eucalyptus grandis leaves, 45g each of Artemisia annua, Schizonepeta tenuifolia, Mentha haplocalyx, Forsythia suspensa, and Pogostemon cablin, and 23g each of Artemisia argyi and Citrus reticulata peel.

4. The method according to claim 1, characterized in that, Preparation of the n-hexane extract of Yin Hu Ganmao San powder: Weigh 1.0 g of Yin Hu Ganmao San powder into an Erlenmeyer flask, add 10 ml of n-hexane, weigh, extract by ultrasonication for 30 min, cool and make up the weight, centrifuge at 8000 rpm for 20 min, take the supernatant and filter it through a 0.22 μm filter membrane for GC-MS analysis.

5. A method for simultaneously determining the content of multiple components in the volatile oil of Yin Hu Ganmao San (a traditional Chinese medicine formula) based on GC-MS combined with MRM, wherein the quality evaluation method includes the following steps: (1) Preparation of volatile oil from Yin Hu Ganmao San: Take 6818g of Pinus massoniana and 6818g of Eucalyptus grandis leaves, crush them, soak them in water at a ratio of 1g:15ml, then steam distill for 2.5h, collect the volatile oil, and store it in a separate container; take 45g each of Artemisia annua, Schizonepeta tenuifolia, Mentha haplocalyx, Forsythia suspensa, and Pogostemon cablin, and 23g each of Artemisia argyi and Citrus reticulata peel, crush them, soak them in water at a ratio of 1g:15ml, then steam distill for 3h, collect the volatile oil, mix the collected volatile oil evenly, take an appropriate amount of the mixed volatile oil, dilute it 20000 times with N,N-dimethylformamide, filter it through a 0.22μm organic phase filter membrane, and then perform GC-MS analysis; (2) The GC analysis procedure for the volatile oil of Yin Hu Ganmao San was as follows: the column temperature was 80℃ for 10 min, the temperature was increased to 150℃ at a rate of 10℃ / min and held for 30 min, the temperature was increased to 200℃ at a rate of 25℃ / min and held for 15 min, the carrier gas was nitrogen with a purity of 99.99%, the split ratio was 10:1, the injection volume was 1 μL, the injection port temperature was 200℃, and the detector temperature was 250℃. (3) Mass spectrometry identification was performed using mass spectrometry libraries (NIST20-1, NIST20-2, NIST20s). Mass spectrometry conditions: the ion source was electron bombardment ionization with an energy of 70 eV, the ion source temperature was 200℃, the interface temperature was 250℃, the full scan mode was m / z 45-500, the electron multiplication voltage was 1.5 kV, and the collision gas was argon with a purity of 99.99%. (4) Combine the mass spectrometry identification results with multiple reaction monitoring for detection and analysis and determination of component content.

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