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GB 31656.1-2021: National food safety standard - Determination of mebendazole and its metabolites residue in fishery products by high performance liquid chromatography
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National food safety standard - Determination of mebendazole and its metabolites residue in fishery products by high performance liquid chromatography
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GB 31656.1-2021
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Basic data | Standard ID | GB 31656.1-2021 (GB31656.1-2021) | | Description (Translated English) | National food safety standard - Determination of mebendazole and its metabolites residue in fishery products by high performance liquid chromatography | | Sector / Industry | National Standard | | Classification of Chinese Standard | X20 | | Word Count Estimation | 7,746 | | Issuing agency(ies) | National Health Commission of the People's Republic of China, State Administration for Market Regulation | GB 31656.1-2021: National food safety standard - Determination of mebendazole and its metabolites residue in fishery products by high performance liquid chromatography
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National food safety standards
Determination of mebendazole and metabolite residues in aquatic products
HPLC
National Standards of People's Republic of China
Released by the National Health Commission of the People's Republic of China
State Administration for Market Regulation
Ministry of Agriculture and Rural Affairs of the People's Republic of China
Foreword
This document complies with the provisions of GB/T 1:1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents"
Drafting:
This document is published for the first time:
1 Scope
This document specifies sample preparation and liquid chromatography for the detection of mebendazole and its metabolites aminomebendazole and hydroxymebendazole residues in aquatic products:
Spectral measurement method:
This document applies to the determination of residues of mebendazole and its metabolites aminomebendazole and hydroxymebendazole in the edible tissues of fish, shrimp and crabs:
Detection:
2 Normative reference documents
The contents of the following documents constitute essential provisions of this document through normative citations in the text: Among them, the cited documents with dates are:
Only the version corresponding to the date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to this document:
document:
GB/T 6682 Rules and test methods for water use in analytical laboratories
GB/T 30891-2014 Sampling specifications for aquatic products
3 Terms and definitions
There are no terms or definitions that need to be defined in this document:
4 Principles
The remaining mebendazole and its metabolites in the sample were extracted with ethyl acetate, degreased with n-hexane, purified with a cationic solid-phase extraction column, and high-performance liquid phase
Determination by chromatography-UV detector and quantification by external standard method:
5 Reagents and materials
The reagents used below are of analytical grade unless otherwise noted, and the water is first-grade water that complies with GB/T 6682:
5:1 Reagents
5:1:1 Acetonitrile (CH₃CN): chromatographically pure:
5:1:2 Methanol (CH₃OH): chromatographically pure:
5:1:3 n-hexane (C₆H14): chromatographically pure:
5:1:4 Ethyl acetate (CH₃COOCH₂CH₃): chromatographically pure:
5:1:5 N,N-dimethylformamide (C₃H₇NO): chromatographically pure:
5:1:6 Phosphoric acid (H₃PO):
5:1:7 Ammonium dihydrogen phosphate (NH₄H₃PO,):
5:1:8 Triethylamine [(C₂H₅)₃N]:
5:1:9 Formic acid (HCOOH):
5:1:10 Ammonia (NH₃·H₂O):
5:2 Standard products
Mebendazole (C16H13N₃O₃, CAS number: 31431-39-7), hydroxymebendazole (5-hydroxymebendazole,
5:3:2 1% formic acid solution: Take 1mL of formic acid, add water to 100mL, and mix well:
5:3:3 0:05mol/L ammonium dihydrogen phosphate-triethylamine solution: Take 5:8g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, add 1mL of triethylamine, and mix:
5:3:4 0:05mol/L ammonium dihydrogen phosphate buffer: Take 2:9g of ammonium dihydrogen phosphate, add 450 mL of water to dissolve, adjust the pH to 2:0 with phosphoric acid, and dilute to 500 mL with water:
5:3:5 5% ammoniated methanol solution: Take 5 mL of ammonia water and 95 mL of methanol, mix well; prepare before use:
5:3:6 Dissolution solution: Take 150mL of N,N-dimethylformamide and dilute to 500mL with 0:05mol/L ammonium dihydrogen phosphate buffer:
5:4 Preparation of standard solution
5:4:1 Standard stock solution (100 μg/mL): Take 10 mg each of mebendazole, aminomebendazole and hydroxymebendazole, and weigh them accurately:
Add 5 mL of formic acid to dissolve, dilute with methanol to a 100 mL volumetric flask, shake well, and prepare standard stock solutions with a concentration of 100 μg/mL:
Store away from light below -18℃, valid for 6 months:
5:4:2 Mix standard intermediate solution: Accurately measure appropriate amounts of mebendazole, aminomebendazole and hydroxymebendazole standard stock solutions, and dilute with methanol:
Release and prepare a mixed standard intermediate solution containing aminomebendazole 5 μg/mL, hydroxymebendazole 2:5 μg/mL and mebendazole 2:5 μg/mL:
Store away from light below -18℃, valid for 3 months:
5:5 Materials
5:5:1 Mixed cationic solid phase extraction column: 60mg/3mL, or equivalent:
5:5:2 Aqueous polysulfone ether needle filter: 0:45μm:
6 Instruments and equipment
6:1 High performance liquid chromatograph equipped with UV detector:
6:2 Analytical balance: sensitivity 0:00001g and 0:01g:
6:3 Centrifuge: 6000r/min:
6:4 Rotary evaporator:
6:5 Solid phase extraction device:
6:6 Ultrasonic cleaning instrument:
6:7 Nitrogen blower:
6:8 Chicken heart bottle: 100mL:
7 Preparation and preservation of specimens
7:1 Preparation of specimens
Prepare samples according to the requirements of Appendix B in GB/T 30891-2014:
a) Take the homogenized test sample as the test sample;
b) Take the homogenized blank sample as the blank sample;
c) Take the homogenized blank sample, add the mixed standard solution of appropriate concentration, and add the sample as a blank:
7:2 Storage of specimens
Stored below -18℃, the validity period is 3 months:
8 Measurement steps
8:1 Extraction
Take 3g of the sample (accurate to ±0:03g) in a 50mL centrifuge tube, add 2mL of water, vortex for 30s to disperse; add ethyl acetate
10 mL, shake for 2 min, ultrasonic for 5 min, centrifuge at 4500 r/min for 10 min, transfer ethyl acetate to a 100 mL chicken heart bottle: Add ethyl acetate to the residue:
Add 10 mL of ester and repeat the extraction twice as described above: Combine the ethyl acetate into a 100 mL chicken heart bottle and rotary evaporate it to dryness at 40°C: Add 80%
Add 3 mL of methanol solution, vortex and mix for 1 min, add 3 mL of n-hexane, mix for 1 min, transfer the solution to a 10 mL centrifuge tube, 6000 r/min
Centrifuge for 5 minutes, remove the n-hexane layer; add 3 mL of n-hexane to the lower layer, and repeat degreasing once: Add 1% formic acid aqueous solution to the lower layer:
3 mL, mix well, centrifuge at 6000r/min for 5min, and set aside the supernatant:
8:2 Purification
The solid-phase extraction column was activated with 3 mL each of methanol and water, and the supernatant was passed through the column; it was rinsed with 4 mL each of water and methanol in sequence, and the effluent was discarded:
Drain: Elute with 5 mL of 5% ammoniated methanol solution: Receive the eluate into a 10 mL centrifuge tube and blow dry with nitrogen at 40°C: Add dissolving solution
Dissolve the residue in 1:0 mL, vortex and mix for 1 min, and filter with an aqueous needle filter into a sample vial for high-performance liquid chromatography measurement:
8:3 Preparation of standard working curve
Precisely measure an appropriate amount of the mixed standard intermediate solution, dilute it with the dissolving solution to prepare mebendazole and hydroxymebendazole concentrations of 0:02 μg/mL, 0:05 μg/mL, 0:1 μg/mL, 0:25 μg/mL, and 0: 5μg/mL and 1:0μg/mL, series with aminomebendazole concentration of 0:04μg/mL, 0:1μg/mL, 0:2μg/mL, 0:5μg/mL, 1:0μg/mL and 2μg/mL Standard working solution for high performance liquid chromatography determination:
Taking the peak area of mebendazole, aminomebendazole and hydroxymebendazole as the ordinate and the corresponding concentration as the abscissa, draw a standard curve and find the regression equation and correlation coefficient: This standard working solution is currently prepared:
8:4 Determination
8:4:1 Liquid chromatography conditions
a) Chromatographic column: C18 column (250mm×4:6mm, 5μm), or equivalent;
b) Mobile phase: A is acetonitrile, B is 0:05 mol/L ammonium dihydrogen phosphate-triethylamine solution, gradient elution conditions are shown in Table 1;
d) Column temperature: 40℃;
e) Injection volume: 30μL;
f) Detection wavelength: 289nm:
8:4:2 Determination method
Take a series of standard working solutions and sample solutions, perform single-point or multi-point calibration, and quantify the standard solutions and sample solutions by chromatographic peak area according to the external standard method:
The response values of medium mebendazole, aminomebendazole and hydroxymebendazole should be within the linear range of instrument detection: Under the above chromatographic conditions
Below, see Appendix A for the liquid chromatogram of the standard solution:
8:5 Blank test
Take a blank sample and perform parallel operations using the same measurement steps except that no standard solution is added:
9 Calculation and presentation of results
The residual amounts of mebendazole, aminomebendazole and hydroxymebendazole in the sample are calculated according to formula (1):
10 Method sensitivity, accuracy and precision
10:1 Sensitivity
The detection limit of mebendazole and hydroxymebendazole in this method is 5 μg/kg, and the limit of quantitation is 10 μg/kg:
The detection limit of aminomebendazole in this method is 10 μg/kg, and the limit of quantitation is 20 μg/kg:
10:2 Accuracy
In this method, mebendazole and hydroxymebendazole are in the range of 10 μg/kg to:200 μg/kg, and aminomebendazole is in the range of 20 μg/kg to 400 μg/kg:
Within the added concentration range, the recovery rate is 70% to 100%:
10:3 Precision
The intra-batch relative standard deviation of this method is ≤15%, and the inter-batch relative standard deviation is ≤15%:
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