SN/T 2012-2019 English PDF

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SN/T 2012-2019: (Detection methods of benzoic acid and sorbic acid in export vinegar. Liquid chromatography and liquid chromatography-mass spectrometry-mass spectrometry)
Status: Valid

SN/T 2012: Historical versions

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
SN/T 2012-2019	459	Add to Cart	4 days	(Detection methods of benzoic acid and sorbic acid in export vinegar. Liquid chromatography and liquid chromatography-mass spectrometry-mass spectrometry)	Valid
SN/T 2012-2007	479	Add to Cart	3 days	Determination of benzoic acid and sorbic acid in vinegar for export and import. Liquid chromatography	Obsolete

Similar standards

GB/T 8967   GB 18187   GB 18186   SN/T 1051   SN/T 4786   SN/T 3936   

Basic data

Standard ID: SN/T 2012-2019 (SN/T2012-2019)
Description (Translated English): (Detection methods of benzoic acid and sorbic acid in export vinegar. Liquid chromatography and liquid chromatography-mass spectrometry-mass spectrometry)
Sector / Industry: Commodity Inspection Standard (Recommended)
Classification of Chinese Standard: X66
Word Count Estimation: 22,274
Date of Issue: 2019-10-25
Date of Implementation: 2020-05-01
Older Standard (superseded by this standard): SN/T 2012-2007
Regulation (derived from): General Administration of Customs Announcement No. 166 of 2019
Issuing agency(ies): General Administration of Customs

SN/T 2012-2019: (Detection methods of benzoic acid and sorbic acid in export vinegar. Liquid chromatography and liquid chromatography-mass spectrometry-mass spectrometry)

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SN/T 2012-2019 Detection method of benzoic acid and sorbic acid in export vinegar Liquid chromatography and liquid chromatography-mass spectrometry/mass spectrometry 1 Scope This standard specifies liquid chromatography detection of benzoic acid and sorbic acid in imported and exported vinegar, and liquid chromatography-mass spectrometry/mass spectrometry detection and verification. method. This standard applies to the determination and confirmation of benzoic acid and sorbic acid in vinegar.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies to this standard quasi. For undated references, the latest version (including all amendments) is applicable to this standard. GB/T 6682 Analytical laboratory water specifications and test methods

3 Method summary

The sample was distilled under acidic conditions, and the distillate was measured by liquid chromatography UV detector or liquid chromatography-mass spectrometry/mass spectrometer. Product quantification.

4 reagents and materials

Unless otherwise specified, all reagents used are analytical grade, and water is first-grade water. 4.1 Methanol. chromatographically pure. 4.2 Acetonitrile. chromatographically pure. 4.3 Citric acid (C6H8O7 · H2O). 4.4 Trisodium citrate (Na3C6H5O7 · 2H2O). 4.5 Tartaric acid. 4.6 Ammonium acetate. chromatographically pure. 4.7 Sodium chloride. 4.8 Sodium bicarbonate. 4.9 citric acid buffer solution (5 mmol/L). Weigh 0.7 g of citric acid (4.3) and 0.6 g of trisodium citrate (4.4) and dissolve in water to the nearest volume of 1 L. 4.10 Tartaric acid (15%). Take 15g of tartaric acid (4.5) and make up to 100mL with water. 4.11 Sodium bicarbonate solution (20g/L). Weigh 2g sodium bicarbonate (4.8), add water to 100mL, and shake to dissolve. 4.12 5mM ammonium acetate solution. Weigh 0.3385g of ammonium acetate (4.6), add water to 1L, and shake to dissolve. 4.13 Sodium benzoate standard material (C6H5COONa, CAS number. 532-32-1), purity ≥99.0%. or benzoic acid (C6H5COOH, CAS number. 65-85-0), a reference material with a purity of ≥99.0%, or certified by the state and awarded a reference material certificate. 4.14 Potassium sorbate reference material (C6H7KO2, CAS number. 590-00-1), purity ≥99.0%; or sorbic acid (C6H8O2, CAS number. 110-44-1), reference materials with a purity of ≥99.0%, or certified by the state and granted a reference material certificate. 4.15 Standard solutions of benzoic acid and sorbic acid (1000 mg/L). Weigh accurately the sodium benzoate (4.13) and potassium sorbate (4.14), respectively. SN/T 2012-2019 The quasi-substances are 0.118 g and 0.134 g (accurate to 0.0001 g), dissolved in water and made up to 100 mL. Store at 4 ° C. When using benzyl For acid and sorbic acid standards, dissolve and make up the volume with methanol. 4.16 Standard mixture of benzoic acid and sorbic acid. Accurately transfer each of the benzoic acid and sorbic acid standard stock solutions (4.15) to 10.0mL and transfer to 100mL. In a volumetric flask, make up to volume. Store at 0 ℃ ～ 4 ℃ for 1 week. 4.17 Blank sample extraction solution. A solution obtained by using a blank sample according to step 6.1. 4.18 Antifoaming agent. Shin-Etsu KM-72GS. 4.19 Filter membrane. 0.45 μm, water system. 4.20 Filter membrane. 0.221 μm, water system.

5 instruments and equipment

5.1 Balance. Sensitivity is 0.1mg and 1mg. 5.2 HPLC. equipped with UV detector. 5.3 High performance liquid chromatography-mass spectrometry/mass spectrometer, equipped with an electrospray ionization source (ESI). 5.4 Distillation device. See Appendix A.

6 Measurement steps

6.1 Treatment of samples Accurately weigh 50.0g sample, add 40g sodium chloride (4.7), 5mL 15% tartaric acid solution (4.10), 1 drop of defoamer (4.18), add Water to about.200mL, after mixing, perform distillation (distillation speed is about 2.5mL/min), collect about 90mL of distillate, make up to volume with water 100mL. After filtering through a 0.45 μm filter, it is determined by liquid chromatography (if confirmed by mass spectrometry, filter through a 0.22 μm filter). 6.2 Determination 6.2.1 Liquid chromatography conditions The liquid chromatography conditions are as follows. a) Chromatographic column. C18 column (150mm × 4.6mm, 5μm, or equivalent); b) mobile phase. methanol. acetonitrile. 5 mmol/L citric acid buffer solution (10.20.70, V/V/V); c) Flow rate. 1.0mL/min; d) detection wavelength. 230nm; e) Column temperature. 30 ° C; f) Injection volume. 20 μL. 6.2.2 HPLC-MS/MS conditions The HPLC-MS/MS conditions are as follows. a) Chromatographic column. C18 column (100mm × 2.1mm, 1.7μm, or equivalent); b) mobile phase. methanol-5mm ammonium acetate solution, the gradient elution procedure is shown in Table 1; Table 1 Gradient elution procedure Time (min) 5mm Ammonium acetate (%) Methanol (%) 0.00 90 10 SN/T 2012-2019 Table 1 (continued) Time (min) 5mm Ammonium acetate (%) Methanol (%) 2.30 30 70 3.0 20 80 3.50 20 80 5.0 90 10 c) Flow rate. 0.30mL/min; d) Column temperature. 35 ° C; e) injection volume. 10 μL; f) ion source. electrospray ion source; g) scanning method. negative ions; h) Detection method. multiple response monitoring (MRM); i) Refer to Appendix B for MS/MS reference conditions. 6.2.3 Determination by liquid chromatography According to the content of benzoic acid and sorbic acid in the sample solution, select a standard mixed working solution with a similar concentration to ensure that the benzoic acid and The response value of citric acid is in the linear range, and the standard working solution and the sample solution are sampled at the same volume for injection. Under the above chromatographic conditions, benzoic acid The reference retention times for sorbic acid and sorbic acid were about 6.5 min and 9.4 min, respectively. Chromatograms of benzoic acid and sorbic acid standard solutions are shown in Appendix C C. 1. 6.2.4 Liquid chromatography-mass spectrometry/mass spectrometry determination and confirmation Determine the standard working solution of the sample and matrix according to the LC-MS/MS conditions. The difference in retention time of the products does not exceed ± 2.5%, all the selected ion pairs appear, and the abundance ratio and concentration of the qualitative ion pairs are equivalent to the matrix standard. The abundance ratio of the working solution is consistent, and the allowable deviation of the abundance ratio does not exceed the range specified in Table 2. It can be determined that there is a corresponding test score in the sample. Precipitate. Refer to Appendix C for the multiple reaction monitoring chart of benzoic acid and sorbic acid standard solutions. 2. Table 2 Maximum allowable deviation of relative ion abundance during qualitative determination Relative abundance (% base peak) Allowable relative deviation ＞ 50% ± 20% ＞ 20% to 50% ± 25% ＞ 10% to 20% ± 30% ≤10% ± 50% 6.2.5 Blank test Except not adding styles, follow the above steps.

7 Results calculation and expression

Chromatographic data processing software external standard method or calculation according to formula (1), the calculation results need to deduct the blank value. SN/T 2012-2019 In the formula. A --- the peak area of benzoic acid or sorbic acid in the sample solution; AS --- peak area of benzoic acid or sorbic acid in standard working solution; The calculation result is represented by the arithmetic mean of the parallel measurement values of the test object. When the calculation result is greater than or equal to 1, it remains valid to three digits Number; when the calculation result is less than or equal to 1, two significant digits are reserved. 8 Limit of quantitation, lower limit of accuracy (recovery rate) 8.1 Low limit of determination The limits of quantification of benzoic acid and sorbic acid in liquid chromatography and liquid chromatography-mass spectrometry/mass spectrometry were both 0.1 mg/kg. 8.2 Recovery rate See Appendix D for the determination of liquid chromatography and liquid chromatography-mass spectrometry/mass spectrometry. SN/T 2012-2019

Appendix A

(Informative appendix) Distillation device diagram ÔµÉÆ ÐÀĹ 250mlÈ½Æ ÀÄ × Ö "Ì Figure A. 1 Distillation device diagram SN/T 2012-2019

Appendix B

(Informative appendix) Mass spectrometer reference conditions B. 1 Mass spectrometer reference conditions a) Capillary voltage. 2.5kV; b) Solvent gas temperature. nitrogen 350 ° C; c) Cone hole back blowing. nitrogen 50L/h; d) Desolvent gas flow rate. 650L/h of nitrogen; e) Ion source temperature. 110 ° C; f) Collision gas. argon 3.2 × 10-4 mbar. Table B. 1 Qualitative, quantitative ion pairing and collision energy of benzoic acid and sorbic acid Target name Qualitative ion pair (m/ｚ) Quantitative ion pair (m/ｚ) Collision gas energy/V Benzoic acid 121.0/77.1a 121.0/77.1.20121.0/121.1 1.2120/120.9 0 Sorbic acid 111.1/80.0a 111.1/80.0 0.2011.1/19.5 91.9 111.1/15.9 9 30 a is a quantitative ion; for different mass spectrometers, there may be differences in the instrument parameters. The mass spectrometer parameters should be optimized to the best before the determination. Non-commercial statement. The reference mass spectrometry conditions listed in Appendix A were performed on a Watters ACCIDIT TQ Detector LC/MS. The tests are listed here. The use of instrument models is for reference only and does not involve commercial purposes. Standard users are encouraged to try different manufacturers or models of instruments. SN/T 2012-2019

Appendix C

(Informative appendix) Standard liquid chromatograms and multiple reaction monitoring (MRM) chromatograms Figure C. 1 Liquid chromatograms of benzoic acid and sorbic acid standards Note. Each peak in the figure is. 1. benzoic acid, 2. sorbic acid Figure C. 2 MRM chromatograms of benzoic acid reference materials Figure C. 3 MRM chromatograms of sorbic acid reference materials SN/T 2012-2019

Appendix D

(Informative appendix) Accuracy (recovery rate) Table D. 1 Recovery of liquid chromatography and liquid chromatography-mass spectrometry/mass spectrometry Name Addition Level (mg/kg) Liquid Chromatography Liquid Chromatography Tandem Mass Spectrometry benzoic acid 0.1 88.0% to 104.0% 82.6% to 100.5% 10 89.0% to 99.4% 85.0% to 95.4% 1000 91.2% to 101.6% 900.2% to 96.6% 2000 90.3% to 100.2% 93.1% to 100.0% Sorbic acid 0.1 83.0% to 103.0% 85.4% to 100.0% 10 87.8% to 97.0% 84.3% to 95.0% 1000 89.5% to 98.2% 86.5% to 98.3% 2000 90.5% to 101.1% 92.2% to 102.1% SN/T 2012-2019 SN/T 2012-2019 SN/T 2012-2019 SN/T 2012-2019 70, 犞/犞/犞); SN/T 2012-2019 0.00 90 10 2.30 30 70 3.0 20 80 3.50 20 80 5.0 90 10 SN/T 2012-2019 ＞ 50% ± 20% ＞ 20% ～ 50% ± 25% ＞ 10% ～ 20% ± 30% ≤10% ± 50% SN/T 2012-2019 SN/T 2012-2019 ÔµÉÆ ÐÀĹ 250mlÈ½Æ ÀÄ × Ö "Ì SN/T 2012-2019 犪 121.0/77.1 20 121.0/121.1 1120. 9/120.9 0 犪 111.1/80.20 20 111.1/95.9 111.1/19.5 9 30 SN/T 2012-2019 SN/T 2012-2019 0.1 88.0% to 104.0% 82.6% to 100.5% 10 89.0% to 99.4% 85.0% to 95.4% 1000 91.2% to 101.6% 900.2% to 96.6% 2000 90.3% to 100.2% 93.1% to 100.0% 0.1 83.0% to 103.0% 85.4% to 100.0% 10 87.8% to 97.0% 84.3% to 95.0% 1000 89.5% to 98.2% 86.5% to 98.3% 2000 90.5% to 101.1% 92.2% to 102.1% SN/T 2012-2019 ......

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