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GB 31658.18-2022: (National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography)
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(National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography)
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GB 31658.18-2022
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Basic data | Standard ID | GB 31658.18-2022 (GB31658.18-2022) | | Description (Translated English) | (National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography) | | Sector / Industry | National Standard | | Classification of Chinese Standard | X04 | | Word Count Estimation | 9,912 | | Date of Issue | 2022-09-20 | | Date of Implementation | 2023-02-01 | | Issuing agency(ies) | National Health Commission of the People's Republic of China, State Administration for Market Regulation | GB 31658.18-2022: (National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography)
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National Health Commission of the People's Republic of China
National Food Safety Standards
Determination of triazine residues in food of animal origin
HPLC
National Standards of People's Republic of China
release
State Administration for Market Regulation
Ministry of Agriculture and Rural Affairs of the People's Republic of China
foreword
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules for Standardization Documents"
drafting.
This document is published for the first time.
National Food Safety Standards
Determination of triazine residues in animal food by high performance liquid chromatography
1 Scope
This document specifies the sample preparation and high performance liquid chromatography detection methods for the detection of triazine residues in animal foods.
This document is applicable to the detection of triazine residues in muscle, liver, kidney tissue, milk and goat milk of cattle and sheep.
2 Normative references
The content in the following documents constitutes the essential provisions of this document through normative references in the text. Among them, the dated reference documents,
Only the version corresponding to the date applies to this document; for undated references, the latest version (including all amendments) applies to this document
document.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Terms and Definitions
This document does not have terms and definitions that need to be defined.
4 principles
The residual triazine in the sample was extracted with acetonitrile water (the residual triazine in milk was extracted with acetic acid acetonitrile solution), weak cation exchange solid phase extraction
The column was purified, determined by high performance liquid chromatography-ultraviolet method, and quantified by external standard method.
5 Reagents and materials
The reagents used in the following are all analytical reagents unless otherwise specified; the water is the first-class water in accordance with the provisions of GB/T 6682.
5.1 Reagents
5.1.1 Methanol (CH3OH). chromatographically pure.
5.1.2 Formic acid (HCOOH). chromatographically pure.
5.1.3 Ammonium formate (CH5NO2). chromatographically pure.
5.1.4 Ammonia (NH3.H2O).
5.1.5 Glacial acetic acid (CH3COOH).
5.2 Solution preparation
5.2.1 60% acetonitrile solution. Take 60mL of acetonitrile, add 40mL of water, and mix well.
5.2.2 0.5% acetic acid in acetonitrile solution. Take 2.5 mL of glacial acetic acid, dilute to 500 mL with acetonitrile, and mix well.
5.2.3 5% ammonia solution. take 5mL of ammonia water, add 95mL of water, and mix well.
5.2.4 Acetic acid methanol solution (pH 7.0). Take 6 mL of glacial acetic acid, add 94 mL of methanol, mix well, adjust the pH to 7.0 ± 0.05 with ammonia water.
5.2.5 0.02mol/L ammonium formate solution (pH4.0). take 1.26g of ammonium formate, add 900mL of water to dissolve, adjust the pH to 4.0±0.0 with formic acid
0.05, dilute with water to 1000mL.
5.3 Standards
Diacetamide triazine amidine (Diminazene acetic acid, C14H15N7.2C4H7NO3, CAS number. 908-54-3), content ≥ 91%.
5.4 Preparation of standard solution
5.4.1 Standard stock solution. Take an appropriate amount of diacetamide triazine standard (equivalent to about 10 mg of triazine), weigh it accurately, add water to dissolve
and dilute to a 10mL brown volumetric flask, and prepare a standard stock solution of triazine with a concentration of 1mg/mL. Store in the dark at 4°C, and the validity period is
1 month.
5.4.2 Standard working solution. Accurately measure 1mL of 1mg/mL standard stock solution, put it in a 100mL brown volumetric flask, dilute with water to the mark,
Prepare the triazine standard working solution with a concentration of 10 μg/mL, store it in the dark at 4°C, and have a validity period of 7 d.
5.5 Materials
5.5.1 Weak cation exchange solid phase extraction column. 60mg/3mL, or equivalent.
5.5.2 Microporous nylon filter membrane. 0.22 μm.
6 Instruments and equipment
6.1 High performance liquid chromatography. equipped with ultraviolet detector or diode array detector.
6.2 Analytical balance. Sensitivity 0.00001g and 0.01g.
6.3 pH meter.
6.4 Vortex mixer.
6.5 Vortex shaker.
6.6 High-speed refrigerated centrifuge. speed ≥ 10000r/min.
6.7 Solid phase extraction device.
7 Preparation and storage of samples
7.1 Preparation of samples
7.1.1 Organization
Take an appropriate amount of fresh or thawed blank or test tissue, mince it, and homogenize it.
a) Take the homogeneous test sample as the test sample;
b) Take a homogeneous blank sample as a blank sample;
c) Take a homogeneous blank sample, add a standard solution of appropriate concentration, and add a sample as a blank.
7.1.2 Milk
Take an appropriate amount of fresh or thawed blank or test milk sample, and mix well.
a) Take the uniformly mixed test sample as the test sample;
b) Take a uniformly mixed blank sample as a blank sample;
c) Take a uniformly mixed blank sample, add a standard solution of appropriate concentration, and add a sample as a blank.
7.2 Storage of samples
Store below -18°C.
8 Measurement steps
8.1 Extraction
8.1.1 Organization
Take 2g of the sample (accurate to ±0.05g), put it in a 50mL polypropylene centrifuge tube, add 18mL of 60% acetonitrile solution, vortex for 1min, and store it on ice.
Adjust the pH to 5.5±0.1 with acetic acid, shake for 10 min, centrifuge at 10,000 r/min for 5 min, take the supernatant, and dilute it with 60% acetonitrile solution to
20.0mL, mix well, take 2.0mL (muscle samples take 10.0mL), set aside.
8.1.2 milk
Take 5g of the sample (accurate to ±0.05g), put it in a 50mL polypropylene centrifuge tube, add 10mL of 0.5% acetic acid acetonitrile solution accurately, vortex
1 min, shake for 10 min, centrifuge at 10000r/min for 10 min, remove all the supernatant, and set aside.
8.2 Purification
Take a weak cation-exchange solid-phase extraction column, and activate it with 3mL of methanol and 3mL of water in turn. Take the spare liquid to pass through the column, and then dissolve it with 5% ammonia water in turn.
Wash with 3 mL of methanol solution and 3 mL of methanol, drain, add 1.0 mL of acetic acid methanol solution (pH 7.0), elute, drain, collect eluate, pass through microporous nylon
filter membrane for determination by high performance liquid chromatography.
8.3 Preparation of standard curve
Precisely measure an appropriate amount of standard working solution, dilute it with acetic acid-methanol solution (pH 7.0), and prepare a concentration of 0.05 μg/mL, 0.1 μg/mL,
0.2μg/mL, 0.5μg/mL, 1μg/mL, 2μg/mL, 5μg/mL series of standard solutions, passed through microporous nylon filter membrane, for HPLC
Chromatographic determination. With triazine chromatographic peak area as the ordinate and standard solution concentration as the abscissa, draw a standard curve. Find the regression equation and
correlation coefficient.
8.4 Determination
8.4.1 Reference conditions for liquid chromatography
a) Chromatographic column. C18 column (250mm×4.6mm, particle size 5μm), or equivalent;
b) Mobile phase. A is 0.02mol/L ammonium formate solution (pH4.0); B is methanol;
c) Gradient elution. see Table 1 for elution conditions;
d) Column temperature. 30°C;
e) Injection volume. 20 μL;
f) Detection wavelength. 370nm.
8.4.2 Determination method
Take the sample solution and the corresponding standard solution for single-point or standard curve calibration, and calculate the peak area according to the external standard method. Standard working solution and sample
The response value of triazine in the solution should be within the linear range of instrument detection. The retention time of triazine in the test sample and the retention time of triazine in the standard solution
The relative deviation of the retention time should be within ±2.5%. The chromatogram of the standard solution is shown in Appendix A.
8.5 Blank test
Take the blank sample, except that no drug is added, the exact same determination steps are used for determination.
9 Calculation and presentation of results
The content of the analyte in the sample is represented by the mass fraction X, and the unit is milligrams per kilogram (mg/kg), calculated according to formula (1).
10 Detection method sensitivity, accuracy and precision
10.1 Sensitivity
The detection limit of this method in beef and mutton is 0.05 mg/kg, and the limit of quantification is 0.1 mg/kg. In bovine liver, bovine kidney, goat liver and goat kidney
The limit of detection was 0.2 mg/kg, the limit of quantification was 0.5 mg/kg, the limit of detection in cow and goat milk was 0.01 mg/kg, the limit of quantification was
0.02mg/kg.
10.2 Accuracy
This method is effective in beef and mutton 0.1mg/kg~1mg/kg, beef liver and sheep liver 0.5mg/kg~24mg/kg, beef kidney and sheep kidney
0.02mg/kg~0.3mg/kg for cow's milk and goat's milk, the recoveries were 60%~110%.
10.3 Precision
In this method, the relative standard deviation within the batch was ≤10%, and the relative standard deviation between batches was ≤10%.
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