GB 23200.115-2018 English PDF

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GB 23200.115-2018: National food safety standard -- Determination of fipronil and its metabolite residues in eggs -- Liquid chromatography -- Mass spectrometry
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.115-2018	159	Add to Cart	3 days	National food safety standard -- Determination of fipronil and its metabolite residues in eggs -- Liquid chromatography -- Mass spectrometry	Valid

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GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.120   GB 23200.121   GB 23200.119   

Basic data

Standard ID: GB 23200.115-2018 (GB23200.115-2018)
Description (Translated English): National food safety standard -- Determination of fipronil and its metabolite residues in eggs -- Liquid chromatography -- Mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 8,813
Date of Issue: 2018-06-21
Date of Implementation: 2018-12-21
Regulation (derived from): National Health and Wellness Commission Announcement No.6 of 2018
Issuing agency(ies): National Health Commission of the People's Republic of China, State Administration for Market Regulation

GB 23200.115-2018: National food safety standard -- Determination of fipronil and its metabolite residues in eggs -- Liquid chromatography -- 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.
National food safety standards Fipronil and its metabolites in eggs Determination of residual amounts Liquid chromatography-mass spectrometry State Administration for Market Regulation Ministry of Agriculture and Rural Affairs of the People's Republic of China National Health Commission of the People's Republic of China

1 Scope

This standard specifies a liquid chromatography-mass spectrometry method for the determination of fipronil and its metabolites residues in eggs: This standard is applicable to the determination of fipronil and its metabolites residues in eggs: 2Normative reference documents The following documents are essential for the application of this document: For dated references, only the dated version applies to this document: For undated referenced documents, the latest version (including all amendments) applies to this document: GB 2763 National Food Safety Standard Maximum Residue Limits of Pesticides in Foods GB/T 6682 Analytical laboratory water specifications and test methods

3 principles

The sample was extracted with acetonitrile, and the extract was purified by dispersive solid-phase extraction, detected by liquid chromatography-mass spectrometry, and quantified by the external standard method:

4 Reagents and materials

Unless otherwise stated, only analytically pure reagents are used in the analysis, and the water is first-grade water specified in GB/T 6682: 4:1 Reagents 4:1:1 Acetonitrile (CH₃CN, CAS number: 75-05-8): chromatographically pure: 4:1:2 Formic acid (HCOOH, CAS number: 64-18-6): chromatographically pure: 4:1:3 Methanol (CH₃OH, CAS number: 67-56-1): chromatographically pure: 4:1:4 Ammonium acetate (CH₃COONH,, CAS number: 631-61-8): chromatographically pure: 4:1:5 Anhydrous magnesium sulfate (MgSO CAS number: 7487-88-9): 4:1:6 Sodium chloride (NaCl, CAS number: 7647-14-5): 4:1:7 Anhydrous sodium sulfate (Na₂SO₄, CAS number: 7757-82-6): 4:2 Solution preparation 4:2:1 Formic acid solution (0:1%): Dilute 1mL of formic acid to 1000mL with water and shake well: 4:2:2 Ammonium acetate-formic acid solution (5mmol/L): Weigh 0:3854g ammonium acetate, dissolve it with 0:1% formic acid solution and dilute it to 1000 mL, shake well: 4:3 Standard products For standard standards of fipronil and its metabolites, see Appendix A, purity ≥95%: 4:4 Preparation of standard solution 4:4:1 Standard stock solution (100mg/L): Accurately weigh 10 ml each of fipronil, fluformonil, fipronil sulfone and fipronil sulfoxide (4:3) mg (accurate to 0:1 mg), dissolve and dilute to 100 mL with acetonitrile, shake well, and prepare a standard stock solution with a mass concentration of 100 mg/L: Store in the dark at -18°C and is valid for 1 year: 4:4:2 Mixed standard intermediate solution (1mg/L): Accurately draw the standard reserves of fipronil, flucarbonitrile, fipronil sulfone and fipronil sulfoxide respectively Dilute 1 mL of each solution (4:4:1) with acetonitrile to 100 mL, shake well, and prepare a 1 mg/L mixed standard intermediate solution: Store in the dark at 0°C to 4°C: The validity period is 1 month: 4:5 Materials 4:5:1 Ethylenediamine-N-propyl silanized silica gel (PSA): 40 μm ~ 60 μm: 4:5:2 Octadecylsilane bonded silica gel (Cg): 40 μm ~ 60 μm: 4:5:3 Microporous filter membrane (organic phase): 0:22μm:

5 instruments

5:1 Liquid chromatography-triple quadrupole mass spectrometer: equipped with ESI source: 5:2 Analytical balance: sensitive to 0:1mg and 0:01g: 5:3 Centrifuge: the rotation speed is not less than 5000 r/min: 5:4 Vortex oscillator: 5:5 oscillator: 5:6 Tissue homogenizer:

6 Sample preparation

6:1 Sample preparation Take 16 fresh eggs (about 1kg), wash and shell them, mix thoroughly with a tissue homogenizer, and put them into a polyethylene bottle: 6:2 Sample storage Store the samples separately for testing and backup at -20°C ~ -16°C:

7 Analysis steps

7:1 Extraction Accurately weigh 5g of the sample (accurate to 0:01g) and place it in a 50mL centrifuge tube, add 20mL of acetonitrile, vortex and mix for 1 min, shake and extract for 5 min, add 2g of sodium chloride and 6g of anhydrous sodium sulfate, vortex for 1 min: Centrifuge at 5000r/min for 5 minutes, and the supernatant needs to be purified: 7:2 Purification Accurately transfer 1 mL of supernatant into a 2 mL polypropylene centrifuge tube, add 50 mg PSA powder, 50 mg C₁s powder and 150 mg anhydrous magnesium sulfate, vortex and mix for 30 s, centrifuge at 5000 r/min for 5 min, and filter the supernatant through 0:22 μm filter: membrane for measurement: 7:3 Instrument reference conditions 7:3:1 Liquid Chromatography Reference Conditions a) Chromatographic column: Cs (2:1mm×100mm, 2:7μm), or one with equivalent performance; b) Column temperature: 35℃; c) Mobile phase: ammonium acetate-formic acid solution (Phase A), methanol (Phase B); d) Flow rate: 0:4mL/min; e) Injection volume: 2μL; f) See Table 1 for mobile phase and gradient elution conditions: 7:3:2 Mass spectrometry reference conditions a) Scanning method: negative ion scanning (ESI-); b) Capillary voltage: 3500V; c) Ion source temperature: 250℃; d) Drying air flow: 7L/min; e) Atomizing gas pressure: 35 psi; f) Sheath gas temperature: 325℃; g) Sheath gas (N₂) flow rate: 11L/min; h) Nozzle voltage: 400V; i) Detection method: multiple reaction monitoring (MRM), the monitoring conditions are shown in Table 2: 7:4 Matrix Mixing Standard Working Curve Accurately draw a certain amount of the mixed standard intermediate solution, and dilute it step by step with the blank matrix extract solution to a mass concentration of 0:001mg/L: Matrix mixed standard working solutions of 0:002mg/L, 0:004mg/L and 0:01mg/L, 0:02mg/L are used for determination by liquid chromatography-mass spectrometry: Draw a standard curve with the pesticide quantitative ion peak area as the ordinate and the pesticide matrix standard solution mass concentration as the abscissa: 7:5 Qualitative and quantitative 7:5:1 Retention time The retention time of the target pesticide chromatographic peak in the test sample is compared with the retention time of the corresponding standard chromatographic peak: The relative error should be within ± Within 2:5%: 7:5:2 Quantitative ions, qualitative ions and product ion abundance ratios When measuring samples under the same experimental conditions, if the retention time of the detected chromatographic peak is consistent with that of the standard sample, and in the mass spectrum of the sample after subtracting the background, both the mass spectrometric quantification and qualitative ions of the target compound appear, and the same detection Batch, for the same compound, if the relative abundance ratio of the qualitative ion and quantitative ion of the target compound in the sample is compared with the matrix standard solution with equivalent mass concentration, and the allowable deviation does not exceed the range specified in Table 3, then it can be judged that the sample contains Target pesticides: Inject the matrix mixed standard working solution and the sample solution into the liquid chromatography-mass spectrometer in sequence: The retention time and qualitative ions are identified, and the quantitative ion peak area is measured: The response value of the pesticide in the sample solution to be tested should be within the range detected by the instrument: Within the linear range of quantitative determination, when exceeding the linear range, appropriate multiple dilutions should be made based on the measured concentration before analysis: 7:6 Parallel test Carry out parallel tests on the same sample according to the provisions of 7:1 to 7:3 and 7:5: 7:7 Blank test Except that no sample is added, parallel operations shall be carried out according to the provisions of 7:1 to 7:3 and 7:5:

8 Result calculation

The amount of each pesticide residue in the sample is expressed as a mass fraction: The unit is expressed in milligrams per kilogram (mg/kg) and is calculated according to formula (1): 10 others The limits of quantification of fipronil, fluformonil, fipronil sulfone and fipronil sulfoxide in this method are all 0:005mg/kg: 11 Spectrum The total ion chromatograms of 0:004mg/L fipronil, flucarbonitrile, fipronil sulfoxide and fipronil sulfone standard solutions are shown in Figure 1: ......

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