UPLC-MS / MS determination method for sweetening agent in electronic cigarette atomized substance

Abstract

The invention discloses a UPLC-MS / MS (Ultra Performance Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) determination method for a sweetening agent in an electronic cigarette compound. The UPLC-MS / MS determination method comprises the following steps: (1) sample pretreatment; (2) carrying out LC-MS / MS analysis conditions; and (3) determining a standard curve and quantifying. According to the method, 34 sweeteners can be simultaneously determined, the detection time is greatly shortened, and the detection efficiency is improved. The UPLC-MS / MS combined technology is adopted, the method has high specificity and sensitivity, and the content of the trace sweetening agent in the electronic cigarette can be accurately measured. The method provides powerful technical support for the quality control and supervision of the electronic cigarette product, and is helpful for guaranteeing the health and safety of consumers.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical analysis, and more particularly to a UPLC-MS / MS determination method for sweeteners in electronic cigarette aerosols. Background Art

[0002] With the increasing popularity of e-cigarette products, the ingredients in e-cigarette liquids are becoming more complex. Sweeteners are important flavoring ingredients, and their types and content have a significant impact on the taste and flavor of e-cigarettes. However, due to the wide variety of sweeteners and the different standards and restrictions for the use of different types of sweeteners in e-cigarettes, how to accurately and quickly determine the content of multiple sweeteners in e-cigarettes has become an important issue in the quality control and supervision of the e-cigarette industry.

[0003] Although traditional sweetener determination methods, such as gas chromatography and liquid chromatography, can meet the determination needs to a certain extent, they often have problems such as cumbersome operation, long detection cycle, and insufficient sensitivity.

[0004] Therefore, it is particularly important to develop an efficient, accurate and rapid method for sweetener determination. Summary of the invention

[0005] In view of this, the purpose of the present invention is to provide a UPLC-MS / MS determination method for sweeteners in electronic cigarette aerosols to solve the deficiencies in the prior art. The present invention is based on a simultaneous determination method of 34 sweeteners in electronic cigarettes using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) to achieve rapid and accurate determination of multiple sweeteners in electronic cigarette liquids, providing strong support for the quality control and supervision of electronic cigarette products.

[0006] In order to achieve the above object, the present invention adopts the following technical solution:

[0007] A UPLC-MS / MS method for determining sweeteners in electronic cigarette aerosols comprises the following steps:

[0008] (1) Sample pretreatment

[0009] Firstly, the electronic cigarette aerosol sample is accurately weighed, then a solvent is added to dissolve or dilute it, and finally filtered or centrifuged to obtain the electronic cigarette aerosol sample solution for LC-MS / MS analysis;

[0010] (2) LC-MS / MS analysis conditions

[0011] Chromatographic conditions: select the chromatographic column, set the mobile phase composition, flow rate, column temperature and gradient elution program;

[0012] Mass spectrometry conditions: electrospray ionization source was used to set the ionization voltage, collision energy and scanning range; the MS / MS mode was used for qualitative and quantitative analysis of target compounds;

[0013] The mobile phase composition is: mobile phase A: 0.1% formic acid 5mM ammonium formate solution, mobile phase B: acetonitrile;

[0014] (3) Standard curve and quantification

[0015] First, prepare the standard working solution of each target compound, determine the response value of the standard working solution under the set LC-MS / MS analysis conditions, and draw a standard curve; then compare the response value of the electronic cigarette aerosol sample solution with the standard curve to calculate the content of each target compound in the sample.

[0016] Preferably, in step (1), the solvent is methanol or ethanol.

[0017] Preferably, the chromatographic column in step (2) is BEH C18 1.7um 2.1*100mm.

[0018] Preferably, the flow rate in step (2) is 0.4 mL / min.

[0019] Preferably, the column temperature in step (2) is 40°C.

[0020] Preferably, the gradient elution program in step (2) is: 0 min, A 85%, B 15%; 0.5 min, A 85%, B 15%; 7.0 min, A 10%, B 90%; 7.1 min, A 85%, B 15%; 10.0 min, A 85%, B 15%.

[0021] Preferably, in step (2), the ionization voltage includes capillary voltage and cone voltage.

[0022] Preferably, the capillary voltage is 2.0 kV in negative mode; and the cone voltage is 20 eV.

[0023] Preferably, the temperature of the electrospray ionization ion source in step (2) is 120°C.

[0024] Preferably, the target compound in step (3) includes: sucralose, neotame, advantame, lactitol, xylitol, sorbitol, acesulfame potassium, cyclamate, saccharin sodium, aspartame, mogroside V, glycyrrhizin, trilobatin, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, steviolbioside, neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperetin, hesperetin dihydrochalcone, hesperidin, methyl hesperidin, and hesperetin dihydrochalcone glucoside.

[0025] It can be seen from the above technical solution that compared with the prior art, the present invention has the following beneficial effects:

[0026] 1. Improved detection efficiency: This method can simultaneously measure 34 sweeteners, greatly shortening the detection time and improving detection efficiency.

[0027] 2. Improved detection accuracy and sensitivity: Using UPLC-MS / MS combined technology, this method has high specificity and sensitivity and can accurately determine the content of trace sweeteners in e-cigarettes.

[0028] 3. It helps in the quality control and supervision of e-cigarette products: This method provides strong technical support for the quality control and supervision of e-cigarette products, and helps to protect the health and safety of consumers.

[0029] 4. Expanded the application scope of UPLC-MS / MS technology: This method is not only suitable for the determination of sweeteners in e-cigarettes, but can also be applied to the simultaneous determination of multiple components in other complex samples, providing a new technical means for quality control in the fields of food, medicine, cosmetics, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0031] Figure 1 This is the standard solution spectrum of xylitol, sorbitol, saccharin sodium, aspartame, mogroside V, glycyrrhizin, and trilobatin.

[0032] Figure 2 This is the standard solution spectrum of neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperidin, hesperidin dihydrochalcone, hesperidin, methyl hesperidin, and hesperidin dihydrochalcone glucoside.

[0033] Figure 3 This is the standard solution spectrum of sucralose, neotame, advantame, lactitol, acesulfame potassium, cyclamate, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, and steviolbioside. DETAILED DESCRIPTION

[0034] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. 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.

[0035] Example 1

[0036] This embodiment provides a UPLC-MS / MS determination method for sweeteners in electronic cigarette aerosols, comprising the following steps:

[0037] (1) Sample pretreatment

[0038] Firstly, the electronic cigarette aerosol sample is accurately weighed, then methanol is added to dissolve it, and finally filtered to obtain the electronic cigarette aerosol sample solution for LC-MS / MS analysis;

[0039] (2) LC-MS / MS analysis conditions

[0040] Chromatographic conditions: BEH C18 1.7um 2.1*100mm chromatographic column was selected, and the mobile phase composition was set as follows: mobile phase A: 0.1% formic acid 5mM ammonium formate solution, mobile phase B: acetonitrile; flow rate was 0.4mL / min, column temperature was 40°C; gradient elution program was: 0min, A 85%, B 15%; 0.5min, A 85%, B 15%; 7.0min, A 10%, B 90%; 7.1min, A85%, B 15%; 10.0min, A 85%, B 15%;

[0041] Mass spectrometry conditions: electrospray ionization source temperature was 120°C, capillary voltage was set to 2.0 kV in negative mode, cone voltage was 20 eV, as well as collision energy and scanning range; MS / MS mode was used for qualitative and quantitative analysis of target compounds;

[0042] (3) Standard curve and quantification

[0043] First, prepare standard working solutions of sucralose, neotame, advantame, lactitol, xylitol, sorbitol, acesulfame potassium, cyclamate, saccharin sodium, aspartame, mogroside V, glycyrrhizin, trilobatin, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, stevioside, neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperidin, hesperidin dihydrochalcone, hesperidin, methyl hesperidin, and hesperidin dihydrochalcone glucoside, determine the response values ​​of the standard working solutions under the set LC-MS / MS analysis conditions, and draw a standard curve; then compare the response values ​​of the electronic cigarette aerosol sample solution with the standard curve, and calculate the content of each target compound in the sample.

[0044] Example 2

[0045] This embodiment provides a UPLC-MS / MS determination method for sweeteners in electronic cigarette aerosols, comprising the following steps:

[0046] (1) Sample pretreatment

[0047] First, accurately weigh the electronic cigarette aerosol sample, then add ethanol to dilute it, and finally centrifuge it to obtain the electronic cigarette aerosol sample solution for LC-MS / MS analysis;

[0048] (2) LC-MS / MS analysis conditions

[0049] Chromatographic conditions: BEH C18 1.7um 2.1*100mm chromatographic column was selected, and the mobile phase composition was set as follows: mobile phase A: 0.1% formic acid 5mM ammonium formate solution, mobile phase B: acetonitrile; flow rate was 0.4mL / min, column temperature was 40°C; gradient elution program was: 0min, A 85%, B 15%; 0.5min, A 85%, B 15%; 7.0min, A 10%, B 90%; 7.1min, A85%, B 15%; 10.0min, A 85%, B 15%;

[0050] Mass spectrometry conditions: electrospray ionization source temperature was 120°C, capillary voltage was set to 2.0 kV in negative mode, cone voltage was 20 eV, as well as collision energy and scanning range; MS / MS mode was used for qualitative and quantitative analysis of target compounds;

[0051] (3) Standard curve and quantification

[0052] First, prepare standard working solutions of sucralose, neotame, advantame, lactitol, xylitol, sorbitol, acesulfame potassium, cyclamate, saccharin sodium, aspartame, mogroside V, glycyrrhizin, trilobatin, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, stevioside, neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperidin, hesperidin dihydrochalcone, hesperidin, methyl hesperidin, and hesperidin dihydrochalcone glucoside, determine the response values ​​of the standard working solutions under the set LC-MS / MS analysis conditions, and draw a standard curve; then compare the response values ​​of the electronic cigarette aerosol sample solution with the standard curve, and calculate the content of each target compound in the sample.

[0053] Performance Testing

[0054] 1. Validation report on the determination method of 34 sweeteners in e-cigarette liquid

[0055] 1. Purpose

[0056] By conducting a methodological investigation on the method, the feasibility, accuracy and reliability of the content determination method of 34 sweeteners (sucralose, neotame, advantame, lactitol, xylitol, sorbitol, acesulfame potassium, cyclamate, saccharin sodium, aspartame, mogroside V, glycyrrhizin, trilobatin, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, steviolbioside, neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperetin, hesperetin dihydrochalcone, hesperidin, methyl hesperidin, hesperetin dihydrochalcone glucoside) in e-cigarette liquid were verified, providing an executable procedure for routine testing.

[0057] 2. Scope of application

[0058] It is suitable for the verification of the determination method of sucralose, neotame, advantame, lactitol, xylitol, sorbitol, acesulfame potassium, cyclamate, saccharin sodium, aspartame, mogroside V, glycyrrhizin, trilobatin, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, stevioside, neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperetin, hesperetin dihydrochalcone, hesperetin, methyl hesperidin, and hesperetin dihydrochalcone glucoside in electronic cigarette liquid.

[0059] 3. Inspection method basis

[0060] The detection program is developed in-house.

[0061] 4. Verification Project

[0062] 4.1 Specificity, linearity and range, limit of quantitation (LOQ), limit of detection (LOD), accuracy, precision, and solution stability.

[0063] 4.2 Verification conclusion

[0064] Table 1

[0065]

[0066] 5. Main reagents and instruments

[0067] 5.1. Ultrapure water (made by the company, 20201228, 20201229, 20201230)

[0068] 5.2. Acetonitrile (HPLC) (SupeLco, batch number: JB096830)

[0069] 5.3. Formic acid (KermeL, batch number: 20190807)

[0070] 5.4. Ammonium formate (Sigma, batch number: BCBV1667)

[0071] 5.5. Liquid chromatography-mass spectrometry (triple quadrupole) (Instrument number: RELX-C-088)

[0072] 5.6. Analytical balance (1 / 10,000) (Instrument No.: RELX-C-009)

[0073] 5.7. Micropipette (10-100 μL) (Instrument No.: RELX-C-032)

[0074] 5.8. Micropipette (20-200 μL) (Instrument No.: RELX-C-031)

[0075] 5.9. Micropipette (100~1000μL) (Instrument No.: RELX-C-030)

[0076] 6. Standard substances and solutions

[0077] 6.1. Sucralose (China Food and Drug Administration, 190120-201902, purity 99.9%)

[0078] 6.2. Neohesperidin dihydrochalcone (aLaddin, D1725048, purity 98.0%)

[0079] 6.3. Neotame (Beijing Coast Hongmeng Standard Material Technology Co., Ltd., L493, 1000 μg / mL)

[0080] 7. Detection Methods

[0081] 7.1 Solution preparation (the amount of solution can be adjusted according to actual needs)

[0082] 7.1.1 Sample diluent: ultrapure water.

[0083] 7.1.2 Mobile phase A: 0.1% formic acid 5 mM ammonium formate solution.

[0084] 7.1.3 Mobile phase B: acetonitrile.

[0085] 7.1.4 Preparation of standard curve mother solution: Weigh appropriate amount of each standard substance, add ethanol to dilute and make up to volume, then dilute with ultrapure water. The concentration of neotame, adventitone, lactitol, acesulfame potassium, sodium cyclamate and saccharin sodium is 5 μg / mL, and the concentration of other components is 100 μg / mL.

[0086] 7.1.5 Preparation of standard curve solution:

[0087] Table 2

[0088]

[0089] 7.1.6 Sample solution: weigh 1.0g of the e-cigarette liquid to be tested into a 10mL volumetric flask, add ultrapure water to dilute to the scale, and shake well; take 100μL of the above solution into a 10mL volumetric flask, add ultrapure water to dilute to the scale, and shake well.

[0090] 7.2 Chromatographic conditions

[0091] Table 3

[0092]

[0093] Table 4: Mass spectrometry parameters

[0094]

[0095]

[0096] Table 5: MRM parameters

[0097]

[0098]

[0099] 7.3 Sampling analysis: Sampling analysis: ultrapure aqueous solution, standard curve solution, sample solution, etc.

[0100] 7.4 System suitability acceptance criteria

[0101] The linear correlation coefficient R of each component 2 ≥0.99.

[0102] 8. Verification Procedure

[0103] 8.1. Exclusivity

[0104] 8.1.1 Solution preparation

[0105] Linear solution 3 mixed standard solution;

[0106] Electronic cigarette liquid sample solution: weigh 1.0 g of the electronic cigarette liquid to be tested into a 10 mL volumetric flask, add ultrapure water to dilute to the scale, and shake well to obtain a concentration of 100 mg / mL; take 1000 μL of the above solution into a 10 mL volumetric flask, add ultrapure water to dilute to the scale, and shake well.

[0107] E-cigarette liquid spiked sample solution: Pipette 1000 μL of 100 mg / mL e-cigarette liquid into a 10 mL volumetric flask, add 500 μL of mixed standard solution, and dilute to the mark with ultrapure water solution.

[0108] 8.1.2 Sampling analysis: Inject and analyze the blank solution and the above-mentioned test solution.

[0109] 8.1.3 Acceptable criteria: The blank solution has no interference with the test components; the e-cigarette liquid matrix has no interference with the test components.

[0110] 8.1.4 Experimental Results

[0111] Table 6

[0112]

[0113]

[0114] Conclusion: The blank solution had no interference with the detection components, and the recovery rate of the sample spiked solution was 83.5%-109.6%, which met the acceptable standard. The blank e-cigarette liquid matrix had no interference with the detection components, indicating that the method had good specificity.

[0115] 8.2. Linear

[0116] 8.2.1. Solution preparation:

[0117] See Table 2 for the standard curve solution.

[0118] 8.2.2. Operation method: Inject the linear solutions one by one, and draw the standard curve with the peak area ratio of each component in the linear solution as the ordinate and the concentration of each component in the standard working solution as the abscissa.

[0119] 8.2.3. Acceptable standard: Linear correlation coefficient R of the standard curve of each component 2 ≥0.99

[0120] 8.2.4 Experimental results

[0121] Table 7

[0122]

[0123]

[0124] Conclusion: The minimum linear correlation coefficient of the 34 sweeteners was 0.9906, all of which met the acceptable standard ≥0.99, indicating that the method had a good linear relationship.

[0125] 8.3. Limit of quantitation and limit of detection

[0126] 8.3.1. Solution preparation:

[0127] Quantitation limit test solution: The lowest point of linearity is taken as the quantitation limit test solution.

[0128] Detection limit test solution: Add appropriate amount of ultrapure aqueous solution for dilution, the concentration of neotame, adventitone, lactitol, acesulfame potassium, sodium cyclamate and saccharin sodium is 0.005μg / mL, and the concentration of other components is 0.1μg / mL. The dilution concentration can be adjusted according to the actual test results until the appropriate concentration is found.

[0129] 8.3.2. Acceptable standards:

[0130] The S / N of each component in the quantitative limit solution is ≥10:1

[0131] Detection limit: S / N of each component in the solution ≥ 3:1

[0132] 8.3.3 Experimental results

[0133] in conclusion:

[0134] The minimum S / N in the quantitative limit solution is 17, meeting the requirement of ≥10:1. That is, the quantitative limits of neotame, adventitone, lactitol, acesulfame potassium, sodium cyclamate and saccharin sodium are 0.1μg / mL, and the concentration of other components is 2.0μg / mL

[0135] The minimum S / N in the detection limit solution is 6, meeting the requirement of ≥3:1. That is, the detection limit of neotame, adventitone, lactitol, acesulfame potassium, sodium cyclamate and saccharin sodium is 0.05μg / mL, and the concentration of other components is 1.0μg / mL

[0136] 8.4. Accuracy

[0137] 8.4.1. Solution preparation:

[0138] 8.4.1.1. Sample solution: weigh 1.0 g of the e-cigarette liquid to be tested into a 10 mL volumetric flask, add ultrapure water to dilute to the mark, and shake well; take 100 μL of the above solution into a 10 mL volumetric flask, add ultrapure water to dilute to the mark, and shake well.

[0139] 8.4.1.2. Prepare the accuracy solution according to the following table

[0140] Table 8

[0141]

[0142] 8.4.2. Operation method: Inject the accuracy solutions one by one, record the peak areas, and calculate the concentration of each component in the solution based on the standard curve.

[0143] 8.4.3. Calculation formula:

[0144]

[0145] 8.4.4. Acceptable standard: The recovery rate of each accuracy solution should be within the range of 80% to 120%

[0146] 8.4.5. Experimental results

[0147] Table 9

[0148]

[0149]

[0150]

[0151]

[0152]

[0153] Conclusion: The recoveries of spiked solutions of 34 sweeteners at various concentrations ranged from 80.8% to 118.7%, all meeting the acceptable standards of 80% to 120%.

[0154] 8.5. Precision

[0155] 8.5.1. Repeatability

[0156] Solution preparation: Prepare 6 portions of precision solution according to 8.4.1.2 Accuracy solution-4.

[0157] Operation method: Inject the solutions separately in sequence, record the peak areas, and calculate the concentration of each component in the solution based on the standard curve.

[0158] 8.5.2. Acceptable standard: RSD of the concentration of each component in 6 precision solutions ≤ 10.0%

[0159] 8.5.3. Intermediate precision: Different personnel repeat the operation under 8.5.1.

[0160] 8.5.4. Acceptable standard: RSD of the concentration of each component in 12 precision solutions ≤ 10.0%

[0161] 8.5.5 Experimental results

[0162] Table 10

[0163]

[0164]

[0165]

[0166] Table 11

[0167]

[0168]

[0169]

[0170] in conclusion:

[0171] The maximum RSD of the 34 sweetener concentrations in the six test solutions was 8.3%, all meeting the acceptance standard of ≤10.0%.

[0172] The maximum RSD of the concentrations of 34 sweeteners in the 12 test solutions was 9.3%, which all met the acceptance standard of ≤10.0%, indicating that the method had good precision.

[0173] 8.6. Solution stability

[0174] 8.6.1 Use repeatability SampLe1 as the solution stability test sample, store at 10℃ for 1, 3, and 5 days, and repeat the test to confirm the stability of the solution. The mean of the repeatability test results is used as the result of time 0. The storage time can be adjusted according to the actual situation.

[0175] 8.6.2 Acceptable standard: The ratio of the post-placement test result to the zero-time result should be within the range of 80% to 120%.

[0176] 8.6.3 Experimental Results

[0177] Table 12

[0178]

[0179]

[0180] Conclusion: After the test solution was placed at 10°C for 1 day, the ratio of the concentration of 34 sweeteners in the solution to the zero time ranged from 84.6% to 116.5%, all within the range of 80% to 120%, meeting the acceptable standard. This indicates that the test solution is stable at 10°C for 1 day.

[0181] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0182] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A UPLC-MS / MS method for determining sweeteners in electronic cigarette aerosols, characterized in that: The following steps are involved: (1) Sample pretreatment Firstly, the electronic cigarette aerosol sample is accurately weighed, then a solvent is added to dissolve or dilute it, and finally filtered or centrifuged to obtain the electronic cigarette aerosol sample solution for LC-MS / MS analysis; (2) LC-MS / MS analysis conditions Chromatographic conditions: select the chromatographic column, set the mobile phase composition, flow rate, column temperature and gradient elution program; Mass spectrometry conditions: electrospray ionization source was used to set the ionization voltage, collision energy and scanning range; the MS / MS mode was used for qualitative and quantitative analysis of target compounds; The mobile phase composition is: mobile phase A: 0.1% formic acid 5mM ammonium formate solution, mobile phase B: acetonitrile; (3) Standard curve and quantification First, prepare the standard working solution of each target compound, measure the response value of the standard working solution under the set LC-MS / MS analysis conditions, and draw a standard curve; The response value of the electronic cigarette aerosol sample solution is then compared with the standard curve to calculate the content of each target compound in the sample.

2. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: In step (1), the solvent is methanol or ethanol.

3. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: The chromatographic column in step (2) is BEH C18 1.7um 2.1*100mm.

4. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: The flow rate in step (2) is 0.4 mL / min.

5. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: The column temperature in step (2) is 40°C.

6. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: The gradient elution program in step (2) is: 0 min, A 85%, B 15%; 0.5 min, A 85%, B 15%; 7.0min, A 10%, B 90%; 7.1min, A 85%, B 15%; 10.0min, A 85%, B 15%.

7. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: In step (2), the ionization voltage includes capillary voltage and cone voltage.

8. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 7, characterized in that: The capillary voltage is 2.0 kV in negative mode; the cone voltage is 20 eV.

9. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: The temperature of the electrospray ionization ion source in step (2) is 120°C.

10. The UPLC-MS / MS determination method of sweeteners in electronic cigarette aerosols according to claim 1, characterized in that: The target compound described in step (3) includes: sucralose, neotame, advantame, lactitol, xylitol, sorbitol, acesulfame potassium, cyclamate, saccharin sodium, aspartame, mogroside V, glycyrrhizin, trilobatin, rebaudioside E, rebaudioside O, rebaudioside D, rebaudioside N, rebaudioside M, rebaudioside A, stevioside, rebaudioside F, rebaudioside C, dulcoside A, rubusoside, rebaudioside B, stevioside, neohesperidin dihydrochalcone, naringin, naringin dihydrochalcone, hesperetin, hesperetin dihydrochalcone, hesperetin, methyl hesperidin, and hesperetin dihydrochalcone glucoside.

Images