|
US$159.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
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 | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB 23200.115-2018 | English | 159 |
Add to Cart
|
3 days [Need to translate]
|
National food safety standard -- Determination of fipronil and its metabolite residues in eggs -- Liquid chromatography -- Mass spectrometry
| Valid |
GB 23200.115-2018
|
PDF similar to GB 23200.115-2018
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:
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.115-2018_English be delivered?Answer: Upon your order, we will start to translate GB 23200.115-2018_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of GB 23200.115-2018_English with my colleagues?Answer: Yes. The purchased PDF of GB 23200.115-2018_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|