SN/T 5118-2019 English PDF

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SN/T 5118-2019: (Determination of melamine residues in foodstuffs and feeds for import and export by liquid chromatography-mass spectrometry/mass spectrometry)
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
SN/T 5118-2019	239	Add to Cart	3 days	(Determination of melamine residues in foodstuffs and feeds for import and export by liquid chromatography-mass spectrometry/mass spectrometry)	Valid

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Basic data

Standard ID: SN/T 5118-2019 (SN/T5118-2019)
Description (Translated English): (Determination of melamine residues in foodstuffs and feeds for import and export by liquid chromatography-mass spectrometry/mass spectrometry)
Sector / Industry: Commodity Inspection Standard (Recommended)
Classification of Chinese Standard: B40
Word Count Estimation: 11,189
Date of Issue: 2019-09-03
Date of Implementation: 2020-03-01
Regulation (derived from): Natural Resources Department Announcement No. 7 of 2019
Issuing agency(ies): General Administration of Customs

SN/T 5118-2019: (Determination of melamine residues in foodstuffs and feeds for import and export by 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 melamine residues in foodstuffs and feeds for import and export by liquid chromatography-mass spectrometry/mass spectrometry) ICS 71.040.40B40 People's Republic of China Entry-Exit Inspection and Quarantine Industry Standard SN/T 51118-2019 Determination of melamine residues in food animals and feed for import and export Liquid chromatography-mass spectrometry/mass spectrometry Published.2019-2009-03 2020-03-01 implementation Published 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. Please note that some content of this document may involve patents, and the issuing authority of this document is not responsible for identifying these patents. This standard is proposed and managed by the General Administration of Customs of the People's Republic of China. This standard was drafted. Chongqing Customs of the People's Republic of China, Nanjing Customs of the People's Republic of China. The main drafters of this standard. Xia Mingxing, Li Guangman, Chen Zongxiang, Wang Kaimin, Wu Jie, Tang Baibin, Wang Yu, Hu Shuo, and Li Yingguo. SN/T 5181-2019 ????? ????, ????, ?? Determination of melamine residues in food animals and feed for import and export Liquid chromatography-mass spectrometry/mass spectrometry

1 Scope

This standard specifies the liquid chromatography-mass spectrometry/mass spectrometry method for melamine residues in imported and exported food animals and feed. This standard applies to the determination of melamine in the blood, urine and animal feed of imported and exported food animals (such as pigs, cattle, sheep, rabbits, chickens, ducks). And confirmation.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies to this document. file. For undated references, the latest version (including all amendments) applies to this document. GB/T 6682 Analytical laboratory water specifications and test methods GB/T 14699.1 Feed sampling GB/T.20195 Preparation of animal feed samples

3 Method summary

After the sample was ultrasonically extracted with an acidic methanol aqueous solution, the sample was purified by a mixed cationic solid-phase extraction column, and detected by liquid chromatography-mass spectrometry/mass spectrometry. Confirmed and quantified by internal standard method.

4 reagent materials

Unless otherwise specified, the reagents used are of analytical grade, and the water is first-grade water specified in GB/T 6682. 4.1 Methanol. HPLC grade. 4.2 Acetonitrile. HPLC grade. 4.3 Acetic acid. HPLC grade. 4.4 ammonium acetate 4.5 50% methanol aqueous solution (5 + 5, V/V). Measure 500mL of methanol and 500mL of water and mix. 4.6 95% acetonitrile aqueous solution. Take 50mL of water and 950mL of acetonitrile and mix well. 4.7 5% acetic acid solution. Take 5mL of acetic acid and dissolve in 95mL of water. 4.8 5% ammonia in methanol. Take 5mL of ammonia to dissolve in 95mL of methanol. 4.9 Acidic methanol extraction solution. Add 90 mL of acetic acid to 90 mL of 50% methanol aqueous solution (4.5) and mix. 4.10 5mol/L ammonium acetate solution. Weigh 0.385g of ammonium acetate and dissolve it in 1,000mL of water. 4.11 Reference materials. Melamine (CAS No .. 108-78-1), Melamine internal standard (15N3-Melamine, CAS) No. 2877476-11-3), the purity is greater than 98%. 4.12 Standard stock solution. Accurately weigh 0.1g of melamine standard (accurate to 0.0001g), and fully dissolve it in 50% methanol aqueous solution (4.5). Dissolve, dilute to a 100mL volumetric flask, prepare a standard stock solution with a concentration of 1,000mg/mL, and dissolve the melamine in the isotope. Standard standard 1mg, fully dissolved with 50% methanol aqueous solution (4.5), diluted and fixed in a 10mL volumetric flask, formulated into a concentration of SN/T 5181-2019 ????? ????, ????, ?? For 0.1100 mg/mL standard stock solution, pour the volume of the standard stock solution into brown reagent bottles, and store them in the dark below -18 ° C. 4.13 Standard intermediate stock solution. Accurately transfer 100 μL of melamine standard stock solution (4.12) and 100 μL of melamine internal standard standard stock solution (4.12) in two 100 mL volumetric flasks, dilute to volume with acetonitrile, and separately prepare Melamine standard solution of 1,000 μg/mL and 0.1100 μg/mL melamine isotope internal standard solution were prepared. The solution was placed in a brown reagent bottle and stored under -18 ° C in the dark. 4.14 Standard working solution. Dilute the standard intermediate stock solution (4.13) to a suitable concentration with a 95% acetonitrile aqueous solution (4.6) as required. Standard working curve solution, the reference linear concentration range is 5ng/mL ～ 100ng/mL, the internal standard concentration of melamine isotope is 2ng/mL Ready for immediate use. 4.15 MCX solid phase extraction column (60mg, 3mL) 1) or equivalent. 3mL methanol, 3mL water and 3mL 5% acetic acid in order before use Solution (4.7) was activated. 4.16 Microporous membrane. organic, 0.22 μm.

5 instruments and equipment

5.1 Liquid chromatography-mass spectrometry/mass spectrometer. Power distribution spray ion source (ESI). 5.2 Balance. Sensitivity is 0.0001g and 0.01mg. 5.3 Centrifuge. The speed should not be lower than 8000r/min. 5.4 Vortex mixer. 5.5 Ultrasonic cleaner. 5.6 Solid-phase extraction device. 5.7 Nitrogen blowing instrument.

6 Sample preparation and storage

6.1 Sample collection and preparation 6.1.1 Feed. Collect representative samples in accordance with GB/T 14699.1 and prepare according to GB/T 2095. 6.1.2 Blood. Animal blood is collected with heparin sodium anticoagulant blood collection tubes. The collected amount shall not be less than 10mL, sealed, and marked. 6.1.3 Urine. Collect it with a clean centrifuge tube. The collected amount should not be less than 10mL. After stirring well, seal it and mark it. 6.2 Sample preservation Feed samples were stored at room temperature. Blood and urine samples to be tested were stored at 4 ° C, and blood and urine samples were stored frozen at -18 ° C.

7 Analysis steps

7.1 Extraction Weigh 2g (accurate to 0.01g) samples in 50mL centrifuge tubes, and add 40μL of melamine isotope internal standard solution (4.13, equivalent to melamine isotope internal standard mass of 4ng) and 20mL of acidic methanol extract (4 .9) Vortex and mix for 2 min. Take 10min, freeze centrifuge at 8000r/min at 10 ℃ for 5min, transfer the supernatant 10mL to 15mL test tube, and wait for purification. 1) The MCX solid-phase extraction column is produced by Waters Corporation. This information is provided for the convenience of users of this standard, not the standard management department. Recognition of this product. SN/T 5181-2019 ????? ????, ????, ?? 7.2 purification Transfer the liquid to be purified to the activated MCX solid phase extraction column (4.15), the flow rate cannot exceed 1 drop/s, rinse with 3mL water The centrifuge tube of the sample solution was passed through the column, and the column was washed with 3 mL of methanol (4.1), and finally eluted with 3 mL of a 5% ammonia methanol solution (4.8), and collected. The eluent was dried under nitrogen at 40 ° C, and the residue was fully dissolved in 1.0 mL of a 95% acetonitrile aqueous solution (4.6). After passing through a 0.22 μm filter membrane (4.16), it was subjected to liquid chromatography-mass spectrometry/mass spectrometry Measurement and confirmation. 7.3 Measurement and confirmation 7.3.1 LC-MS/MS Reference Conditions 7.3.1.1 Reference conditions for liquid chromatography The reference conditions are as follows. a) Chromatographic column. HILIC column, 100mm × 2.1mm (inner diameter), 3μm, or equivalent. b) Mobile phase. B. 5 mmol/L ammonium acetate solution (4.10). A. acetonitrile (4.2). See Table 1 for gradient elution procedure. c) Flow rate. 0.4mL/min. c) Column temperature. 40 ° C. d) Injection volume. 5 μL. Table 1 Mobile phase and gradient elution procedure Time (min) Flow rate (ml/min) 5mmol/L ammonium acetate solution (A)% Acetonitrile (B)% 0 0.4 5 95 1 0.4 5 95 4 0.4 40 60 6 0.4 40 60 6.1 0.4 5 95 10 0.4 5 95 7.3.1.2 Mass spectrometry reference conditions The reference conditions are as follows. a) Ion source. Electrospray ion source (ESI). b) scanning method. positive ion; c) Monitoring method. multiple response monitoring (MRM); d) The atomizing gas (GS1), curtain gas (CUR), auxiliary gas (GS2), and collision gas (CAD) are all high-purity nitrogen or other suitable gases; Before use, the gas flow rate, ion source temperature, and electrospray voltage should be set to appropriate values, so that the sensitivity of the mass spectrometer can meet the detection requirements. See Appendix A for detailed conditions; e) The de-clustering voltage (DP), collision chamber inlet voltage (EP), collision voltage (CE), and collision chamber outlet voltage (CXP) should be optimized to the best Conditions, monitoring ions and quantifier ions, see Appendix A for detailed conditions. 7.3.2 Quantitative determination According to the content of the test substance in the sample, prepare a standard working solution with a suitable response value for chromatographic analysis. The standard curve working solution should have The five concentration levels should include the zero point. The response value of melamine in the standard working solution and the test solution should be within the linear response range of the instrument. Such as SN/T 5181-2019 ????? ????, ????, ?? If the content of the analyte in the sample exceeds the linear range of the standard curve, dilute it with a 95% acetonitrile aqueous solution (4.6) to an appropriate concentration and analyze. above The melamine retention time is 2.80 min under the above chromatographic conditions. The melamine standard solution's multiple reaction monitoring (MRM) chromatogram is shown in the appendix. Record B. 7.3.3 Qualitative analysis Determine the sample and standard working solution according to the conditions of liquid chromatography-mass spectrometry/mass spectrometry. The consistency of the product is the same, and the retention time deviation is within 5%. The relative abundance of the qualitative ion pair is a table of the percentage of intensity relative to the abundance of the strongest ion. It should be consistent with the relative abundance of a standard working solution with a fairly standard concentration. The allowable deviation of the relative abundance does not exceed the range specified in Table 2. The corresponding test object exists in the broken sample. Table 2 Maximum allowable deviation of relative ion abundance during qualitative confirmation Relative ion abundance /% ＞ 50 ＞ 20 ～ 50 ＞ 10 ～ 20 ＜ 10 Allowable relative deviation /% ± 20 ± 25 ± 30 ± 50 7.4 Blank test Except for not adding samples, all operations are carried out according to the above operation steps.

8 Results calculation and expression

Use the instrument software to process the data or draw a standard curve according to the internal standard method. The chromatographic peak area ratio of each standard solution to the internal standard solution is horizontal. Coordinate, draw the standard curve with the concentration ratio of each standard solution and internal standard solution as the ordinate, and compare the peak area ratio of the analyte in the sample to the internal standard The value is substituted into the curve equation, and the concentration ratio of the analyte in the sample to the internal standard is calculated. Since the concentration of the internal standard is known, the analyte in the sample is obtained. Concentration C, substituted into formula (1), the calculation result must be deducted from the blank value. In the formula. X --- content of test substance in sample, unit is microgram per kilogram (μg/kg); C --- solution concentration of test substance obtained from standard curve, unit is microgram per liter (μg/L) C0 --- the solution concentration of the test substance in the blank test obtained from the standard curve, the unit is micrograms per liter (μg/L); 犞 --- the final constant volume of the sample solution, the unit is milliliters (mL); The result retains three significant digits. 九 Determination of low limit and recovery 9.1 Low limit of determination (LOQ) The determination of this method is low. the detection limits in blood, urine and animal feed of food animals (such as pigs, cattle, sheep, rabbits, chickens, ducks) are all It is 10 μg/kg. 9.2 Recovery rate This method is used to test the recovery rate of blood, urine, animal feed and other substrates of food animals (such as pigs, cattle, sheep, rabbits, chickens, ducks). See Appendix C for recovery data. SN/T 5181-2019 ????? ????, ????, ?? 10 precision The absolute difference between the two independent results obtained under repeatability conditions does not exceed 10% of the arithmetic mean. SN/T 5181-2019 ????? ????, ????, ??

Appendix A

(Informative appendix) Mass reference conditions 2) Reference MS conditions a) Electrospray voltage (IS). 5500V. b) Impact gas pressure (CAD). Medium; c) Atomizing gas pressure (GS1). 40Psi; d) Curtain gas pressure (CUR). 25Psi; e) Auxiliary gas pressure (GS2). 70Psi; f) Ion source temperature (TEM). 650 ° C; g) For monitoring ion pairs, decluster voltage (DP), collision cell inlet voltage (EP), collision voltage (CE), and collision cell outlet voltage (CXP), see Table A. 1. Table A. 1 Qualitative and quantitative transitions and CE, DP, EP, CXP reference values Compound parent ion (Q1) detection mode ion (Q3) CEV DP EP CXP Melamine 127.0 Positive ion 85.0  40 44 10 5 68.0 62 44 10 5 15N3-melamine Amine internal standard 130.0 Positive ion 87.0 28 60 10 5 Note. The ions with gadolinium in the table are quantitative ions. For different mass spectrometers, the parameters of the instrument may differ. The mass spectrometer parameters should be optimized to the best before the determination. 2) Non-commercial statement. The reference mass spectrometry conditions listed in Appendix A were completed on an ABAPI4000/TRAP LC/MS instrument. The tests are listed here. The instrument model is for reference only and does not involve commercial purposes. Standard users are encouraged to try different manufacturers or models of instruments. SN/T 5181-2019 ????? ????, ????, ??

Appendix B

(Informative appendix) Multi-reaction monitoring (MRM) chromatograms of melamine standard and isotope internal standard solutions SN/T 5181-2019 ????? ????, ????, ??

Appendix C

(Informative appendix) Experimental data of melamine addition recovery in different matrices Matrix addition level μg/kg Recovery rate % Substrate Add level μg/kg Recovery rate Pig blood 10 89.2 to 112.0 20 90.5 to 100.0 100 86.7 to 94.0 2500 108.0 to 113.0 Rabbit blood 10 99.6 to 109.6 20 95.3 to 101.8 100 96.2 to 103.7 2500 97.7 to 112.0 Cow blood 10 99.5 to 110.0 20 91.9 to 101.0 100 93.3 to 103.2 2500 103.9 to 110.9 Urine 10 85.7 to 98.5 20 94.3 to 107.3 100 93.1 to 102.7 2500 96.3 to 99.8 Sheep blood 10 91.5 to 99.5 20 90.3 to 94.2 100 90.8 to 96.8 2500 98.4 to 106.9 Pellet feed 10 99.6 to 109.6 20 97.3 to 100.8 100 94.0 ～ 102.0 2500 93.1 to 97.7 Chicken blood 10 94.0 to 101.0 20 97.0 to 101.5 100 98.4 to 103.4 2 500 100.9 to 103.9 Premix feed 10 98.7 to 109.7 20 98.4 to 107.9 100 99.1 to 116.1 2 500 100.8 to 103.8 Duck blood 10 96.9 to 103.9 20 97.0 to 109.5 100 107.7 to 110.7 2500 93.1 to 97.61 Concentrated feed 10 95.8 to 106.8 20 96.9 to 10.4 100 101.5 to 105.5 2500 94.5 to 101.9 SN/T 5181-2019 ????? ????, ????, ?? ......

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