GB 31657.1-2021 English PDF

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GB 31657.1-2021: National food safety standard - Determination of Tau-fluvalinate residue in honey and royal jelly by gas chromatography method
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Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 31657.1-2021	119	Add to Cart	3 days	National food safety standard - Determination of Tau-fluvalinate residue in honey and royal jelly by gas chromatography method	Valid

Similar standards

GB 31650.1   GB/T 37517   GB/T 30636   GB 31656.14   GB 31657.3   GB 31657.2   

Basic data

Standard ID: GB 31657.1-2021 (GB31657.1-2021)
Description (Translated English): National food safety standard - Determination of Tau-fluvalinate residue in honey and royal jelly by gas chromatography method
Sector / Industry: National Standard
Classification of Chinese Standard: X04
Word Count Estimation: 6,615
Issuing agency(ies): National Health Commission of the People's Republic of China, State Administration for Market Regulation

GB 31657.1-2021: National food safety standard - Determination of Tau-fluvalinate residue in honey and royal jelly by gas chromatography method

---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.
National food safety standards Fluvalinate residues in honey and royal jelly Determination of gas chromatography 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: National food safety standards Determination of fluvalinate residues in honey and royal jelly by gas chromatography

1 Scope

This document specifies the sample preparation and gas chromatographic determination methods for the detection of fluvalinate residues in honey and royal jelly: This document is applicable to the determination of fluvalinate residues in honey and royal jelly:

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 Specifications and test methods for water used in analytical laboratories

3 Terms and definitions

There are no terms or definitions that need to be defined in this document:

4 Principles

The remaining fluvalinate in the sample was dissolved in water, extracted with n-hexane-acetone solution, and purified with a Florisil solid-phase extraction column, using the configuration Determination by gas chromatography with electron capture detector and quantification by external standard method:

5 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade and the water is first-grade water that complies with GB/T 6682: 5:1 Reagents 5:1:1 Acetone (CH3COCH3): chromatographically pure: 5:1:2 n-hexane (C6H14): chromatographically pure: 5:2 Solution preparation 5:2:1 n-hexane-acetone solution (1:1): Take equal volumes of n-hexane and acetone and mix well: 5:2:2 n-hexane-acetone solution (95∶5): Take 5mL of acetone and 95mL of n-hexane and mix well: 5:3 Standard products Fluvalinate (tau-fluvalinate, C26H22ClF3N2O3, CAS number: 102851-06-9): content ≥ 98:0%: 5:4 Preparation of standard solution 5:4:1 Standard stock solution: Take 10 mg of fluvalinate reference substance, weigh it accurately, dissolve it with n-hexane and dilute it to a volume of 100 mL: bottle, prepare a standard stock solution with a concentration of 100 μg/mL: Store at 0°C ~ 5°C, and is valid for 6 months: 5:4:2 Standard working solution: Precisely measure an appropriate amount of standard stock solution, dilute it with n-hexane, and prepare a concentration of 10 μg/L, 20 μg/L, 50μg/L, 100μg/L,:200μg/L and 500μg/L series standard working solutions: Ready for use: 5:5 Materials Florisil solid phase extraction column: 1g/6mL, or equivalent:

6 Instruments and equipment

6:1 Gas chromatograph: equipped with electron capture detector: 6:2 Analytical balance: sensitivity 0:00001g and 0:01g: 6:3 Vortex mixer: 6: Centrifuge: 6:5 Rotary evaporator: 6:6 Solid phase extraction device: 6:7 Nitrogen blower: 7: Preparation and preservation of samples 7:1 Preparation of samples Honey: Stir the test sample evenly; for crystallized samples, place them in a water bath not exceeding 60°C to dissolve them in a sealed state, and stir Mix evenly and quickly cool to room temperature: Separate about 150g as a sample, place it in a sample bottle, seal it, and mark it: Royal jelly: Stir the test sample evenly; for frozen test samples, stir evenly after thawing completely at room temperature: Separate about 150g: As a test material, place it in a sample bottle, seal it, and mark it: 7:2 Preservation of samples Honey: Store at room temperature: Royal jelly: Store below -18℃:

8 Measurement steps

8:1 Extraction Take 5g of honey (accurate to ±0:02g) [2g of royal jelly (accurate to ±0:02g)], put it into a 50mL stoppered polypropylene centrifuge tube, and add water 10 mL, vortex and mix for 1 min to dissolve: Add 20 mL of n-hexane-acetone solution (1:1), vortex for 3 min, and centrifuge at 3000 r/min for 5 min: Take the upper layer into a 150 mL chicken heart bottle: Repeat the extraction once with 20 mL of n-hexane-acetone solution (1:1), combine the upper layers, and decompress in a 40°C water bath: Concentrate to nearly dryness, add 3 mL of n-hexane to dissolve, and set aside: 8:2 Purification The Florisil solid-phase extraction column was activated with n-hexane-acetone solution (95:5) and 5 mL of n-hexane in sequence: Pass the reserve solution through the column, and then use normal hexane: Wash the chicken heart bottle with 3 mL of hexane, pass the washing liquid through the column, and discard this part of the effluent: Elute with 10 mL of n-hexane-acetone solution (95:5), and collect the washing liquid: Deliquidate, blow to dryness with nitrogen in a 40°C water bath, redissolve with 1:0 mL of n-hexane, and use for gas chromatography measurement: 8:3 Preparation of standard working curve Accurately draw an appropriate amount of fluvalinate standard working solution and inject samples respectively: Take the concentration of the standard working solution as the abscissa and the peak area as the vertical axis: mark and draw the standard working curve: 8: Measurement 8:4:1 Gas Chromatography Reference Conditions a) Chromatographic column: VFＧ1MS (100% dimethylpolysiloxane) quartz capillary column (30m×0:0:25mm×0:025m), or equivalent By; b) Carrier gas: nitrogen, purity ≥99:999%; c) Inlet temperature: 280℃; d) Detector temperature: 300℃; e) Column temperature: initial temperature is 80°C, hold for 1 minute, increase temperature to:200°C at 30°C/min, hold for 1 minute, and then increase temperature at 10°C/min: to 280℃, keep for 6 minutes; f) Carrier gas flow rate: 1:0mL/min; g) Injection volume: 1μL; h) Injection method: Splitless injection, open the split valve after 1 minute: 8:4:2 Measurement method Take the sample solution and the corresponding standard solution, perform single-point or multi-point calibration, quantify it based on the chromatographic peak area, and calculate it according to the external standard method: The standard solution and The response value of fluvalinate in the sample solution should be within the linear range of the instrument detection: Under the above chromatographic conditions, the chromatogram of the standard solution is shown in the attachment: Record A: 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 amount of the test substance in the sample is calculated according to the standard curve or formula (1): 10 Sensitivity, accuracy and precision of detection methods 10:1 Sensitivity The detection limits of fluvalinate in honey and royal jelly in this standard method are 2 μg/kg and 4 μg/kg respectively: In this standard method, the quantification limits of fluvalinate in honey and royal jelly are 5 μg/kg and 10 μg/kg respectively: 10:2 Accuracy The recovery rate of fluvalinate in honey at the addition level of 5 μg/kg~100 μg/kg is 70%~120%: The recovery rate of fluvalinate in royal jelly at the addition level of 10 μg/kg to 100 μg/kg is 70% to 120%: 10:3 Precision The intra-batch relative standard deviation of this method is ≤20%, and the inter-batch relative standard deviation is ≤20%: ......

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