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(Determination of Aminopyralid and Amilopic Acid Residues in Exported Food Liquid Chromatography-Mass Spectrometry / Mass Spectrometry)
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Basic data
| Standard ID | SN/T 5219-2019 (SN/T5219-2019) |
| Description (Translated English) | (Determination of Aminopyralid and Amilopic Acid Residues in Exported Food Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.050 |
| Word Count Estimation | 12,170 |
| Date of Issue | 2019 |
| Date of Implementation | 2020-07-01 |
| Issuing agency(ies) | General Administration of Customs |
SN/T 5219-2019: (Determination of Aminopyralid and Amilopic Acid Residues in Exported Food Liquid Chromatography-Mass Spectrometry / Mass Spectrometry)
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of picloram, aminopyralid residues in foods tuffs for export-
LC-MS/MS method
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
2019-12-27 release
2020-07-01 Implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organization of this standard. Shenzhen Customs of the People's Republic of China.
The main drafters of this standard. Wu Fengqi, Zhao Qionghui, Chen Bo, Wu Weidong, Jin Baohui, Zhang Jianying, Jin Xiaolei, Liang Shuwen.
Determination of Ampilloic Acid and Clinopical Acid Residues in Exported Food
Liquid chromatography-mass spectrometry/mass spectrometry
1 Scope
This standard specifies the sample preparation and liquid chromatography-mass spectrometry/mass spectrometry methods for amlpicolinic acid and clopyralid in exported food.
This standard applies to Chinese cabbage, spinach, tomatoes, Chinese kale, apples, bananas, dragon fruit, pears, rice, wheat, pork,
The determination and confirmation of the residues of amphipialic acid and clopyralic acid in foods such as beef, chicken, shrimp, and crucian.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Method summary
After extracting the aminopyridine acid and the aminopyridine acid in the sample with acidified acetonitrile, the modified QuEChERS (150 mg C18
900 mg Na2SO4) reagent, after purifying the extract, the liquid chromatography tandem mass spectrometer was used for qualitative and quantitative analysis.
Standard method for quantification.
4 Reagents and materials
Unless otherwise specified, the reagents used are all analytically pure, and the water is first-grade water that meets the requirements of GB/T 6682.
4.1 Acetonitrile. chromatographically pure.
4.2 Methanol. chromatographically pure.
4.3 Formic acid.
4.4 n-hexane.
4.5 Anhydrous magnesium sulfate.
4.6 C18 powder.
4.7 Sodium chloride.
4.8 Ammonium acetate.
4.9 Anhydrous sodium sulfate.
4.10 Apiclopyridine (Picloram, C6H3Cl3N2O2, CAS No. 1918-02-1). the purity is greater than or equal to 99.0%.
4.11 Aminopyralid (Aminopyralid, C6H4Cl2N2O2, CAS No. 150114-71-9). The purity is greater than or equal to 99.0%.
4.12 Standard stock solution. accurately weigh out 10 mg of shampyridine acid (4.10) and shampyridine acid (4.11) respectively, and use methanol (4.2)
Dissolve and dilute to 10 mL. Store in the dark at -18°C. The shelf life is 6 months.
4.13 Mixed standard solution. Pipette 100 µL of each substance standard stock solution (4.12), add the blank matrix extract to make the volume up to 10 mL,
Store in the dark at -18℃, and the shelf life is 1 month.
4.14 Microporous membrane. 0.22µm, organic.
5 Apparatus and equipment
5.1 Liquid chromatography tandem mass spectrometer. equipped with an electrospray ion source (ESI).
5.2 Analytical balance. Sensitivity is 0.1 mg and 0.01 g respectively.
5.3 Homogenizer.
5.4 High-speed centrifuge. the speed is not less than 9 500 r/min.
5.5 Nitrogen blowing instrument.
5.6 Vortex mixer.
5.7 Organize the masher.
6 Sample preparation and storage
6.1 Sample preparation
Take 500 g of a representative sample, use a tissue masher to process the sample into a slurry, mix well, put it into a clean sample container, and seal it.
And mark it.
6.2 Sample storage
The samples should be frozen and stored below -18°C.
During the operation of sample preparation and storage, the samples should be prevented from being contaminated or from changing the content of residues.
6.3 Extraction
6.3.1 Fruit and vegetable samples
Weigh 10.0 g of the sample, accurate to 0.01 g, and place it in a 50 mL centrifuge tube, add 10 mL of 1% formic acid acetonitrile, 9 500 r/min
After 5 min, add 4g of anhydrous methyl sulfate (4.5) and 1g of sodium chloride (4.7), vortex for 10 min, and centrifuge at 9 500 r/min for 5 min.
6.3.2 Grain samples
Weigh 5.0 g of the sample, accurate to 0.01 g, place it in a 50 mL centrifuge tube, add 3 mL of water, vortex to soak the sample, add
10 mL of 1% formic acid acetonitrile, 9 500 r/min, homogenize for 5 minutes, then add 4 g of anhydrous sulfuric acid (4.5), 1 g of sodium chloride (4.7), and vortex.
Shake for 10 min, centrifuge at 9 500 r/min for 5 min.
6.3.3 Meat samples
Weigh 2.0 g of the sample, accurate to 0.01 g, place it in a 50 mL centrifuge tube, add 2 mL of 5 mmoL/L ammonium acetate buffer, and vortex
After spin-soaking the sample, add 10 mL of 5% formic acid acetonitrile and 5 mL of acetonitrile saturated n-hexane, homogenize at 9 500 r/min for 5 minutes, and then add
4g MgSO4, 1g NaCl, vortex for 10 min, centrifuge at 9 500 r/min for 5 min.
6.4 Purification
6.4.1 Fruit and vegetable samples
Take 6 mL of the supernatant and add 15 mL pre-added with 150 mg of C18 powder (4.6) and 900 mg of anhydrous sodium sulfate (4.9).
In the heart tube, vortex for 3 min, and centrifuge at 9 500 r/min for 5 min. Pipette 1 mL of the supernatant into a 15 mL centrifuge tube, and blow dry with nitrogen.
Dilute the volume to 1 mL with a 10% methanol aqueous solution, vortex to mix, and pass through a 0.22 µm microporous membrane (4.14) for determination by liquid chromatography tandem mass spectrometer.
6.4.2 Grain samples
Take 6 mL of the supernatant and add 15 mL pre-added with 150 mg of C18 powder (4.6) and 900 mg of anhydrous sodium sulfate (4.9).
In the heart tube, vortex for 3 min, and centrifuge at 9 500 r/min for 5 min. Pipette 2 mL of the supernatant into a 15 mL centrifuge tube, blow dry with nitrogen, and use
The volume of 10% methanol aqueous solution was adjusted to 1 mL, vortexed to mix, and passed through a 0.22 µm microporous membrane (4.14) for determination by liquid chromatography tandem mass spectrometer.
6.4.3 Meat samples
Take 6 mL of the supernatant and add 15 mL pre-added with 150 mg of C18 powder (4.6) and 900 mg of anhydrous sodium sulfate (4.9).
In the heart tube, vortex for 3 min, and centrifuge at 9 500 r/min for 5 min. Pipette 5 mL of the supernatant into a 15 mL centrifuge tube, and blow dry with nitrogen.
Dilute the volume to 1 mL with 10% methanol aqueous solution, add 2 mL of acetonitrile saturated n-hexane, vortex to mix, centrifuge at 9 500 r/min for 5 min,
Pass the 0.22 µm microporous filter membrane (4.14) for determination by liquid chromatography tandem mass spectrometer.
7 Determination
7.1 Liquid chromatography/mass spectrometry conditions
7.1.1 Chromatographic column. Eclipse Plus C18 chromatographic column, 50 mm×2.1 mm (inner diameter), particle diameter 1.8 µm or equivalent.
7.1.2 Column temperature. 30 ℃.
7.1.3 Injection volume. 5 µL.
7.1.4 Mobile phase. A is 0.2% formic acid, 2 mmoL/L ammonium acetate aqueous solution, and B is methanol (4.2).
7.1.5 Flow rate. 0.3 mL/min.
7.1.6 Gradient. See Appendix A, Table A.1.
7.1.7 Mass spectrometry conditions. see Appendix A, Table A.2.
7.2 Liquid chromatography/mass spectrometry detection
Under the best working conditions of the instrument, inject the matrix standard calibration solution, taking the peak area of the analyte as the ordinate, the matrix calibration solution
As the ordinate, draw a standard working curve. Use the standard working curve to quantify the sample, and the sample solution to be tested contains amlpicolinic acid and closampidine
The response value of the acid should be within the linear range of the instrument detection. Under the above chromatographic and mass spectrometry conditions, the mass chromatogram of the standard substance multi-reaction monitoring
See Appendix B.
7.3 Qualitative Liquid Chromatography/Mass Spectrometry
If there are chromatographic peaks in the mass chromatograms of the sample solution and the standard working solution at the same retention time, the allowable deviation is less than ±2.5%,
If the abundance ratio of the selected ion and the corresponding ion abundance ratio of the standard product are within the allowable range (see Table 1 for the allowable range), it can be judged
The corresponding analyte is present in the sample. Under the conditions of 7.1, the liquid chromatography-mass spectrometry multi-reaction monitoring phase of amlodipic acid and clopyralid
The maximum allowable deviation of ion abundance is shown in Table 2.
7.4 Blank test
Except that no sample is added, all are carried out according to the above-mentioned measuring conditions and operation steps.
8 Calculation and expression of results
Use the external standard method in the chromatographic data processing software or formula (1) to calculate the residual amount of the drug in the sample.
X--The content of the component to be tested in the sample, in micrograms per kilogram (µg/kg);
c-The content of the analyte in the sample solution obtained from the matrix standard curve, in nanograms per milliliter (ng/mL);
V--The constant volume of the sample, the unit is milli...
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