GB 31656.4-2021 English PDFUS$139.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 31656.4-2021: National food safety standard - Determination of chlorpromazine residue in fishery products by liquid chromatography-tandem mass spectrometric method Status: Valid
Basic dataStandard ID: GB 31656.4-2021 (GB31656.4-2021)Description (Translated English): National food safety standard - Determination of chlorpromazine residue in fishery products by liquid chromatography-tandem mass spectrometric method Sector / Industry: National Standard Classification of Chinese Standard: X20 Word Count Estimation: 7,776 Issuing agency(ies): National Health Commission of the People's Republic of China, State Administration for Market Regulation GB 31656.4-2021: National food safety standard - Determination of chlorpromazine residue in fishery products by liquid chromatography-tandem mass spectrometric 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 Determination of chlorpromazine residues in aquatic products Liquid chromatography-tandem mass spectrometry 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 ForewordThis 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 chlorpromazine residues in aquatic products by liquid chromatography-tandem mass spectrometry1 ScopeThis document specifies the sample preparation and liquid chromatography-tandem mass spectrometry determination methods for the detection of chlorpromazine residues in aquatic products: This document is applicable to the detection of chlorpromazine residues in edible tissues of fish, shrimp and crabs:2 Normative reference documentsThe 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 GB/T 30891-2014 Sampling specifications for aquatic products3 Terms and definitionsThere are no terms or definitions that need to be defined in this document:4 PrinciplesThe remaining chlorpromazine in the sample was extracted with acetonitrile, purified with a mixed cationic solid-phase extraction column, and measured by liquid chromatography-tandem mass spectrometry, using the internal standard method: Quantitative:5 Reagents and materialsThe 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 Formic acid (HCOOH): chromatographically pure: 5:1:4 Ammonium acetate (NH₄C₂H₃O₂): 5:1:5 Ammonia (NH₃·H₂O): 5:2 Standard products 5:3 Solution preparation 5:3:1 5% ammoniated methanol solution: Take 5 mL of ammonia water and 95 mL of methanol, and mix well: 5:3:2 2mmol/L ammonium acetate solution: Take 0:154g of ammonium acetate, add 1mL of formic acid, dissolve with appropriate amount of water and dilute to 1000mL: 5:3:3 30% methanol-ammonium acetate solution: Take 30 mL of methanol and 70 mL of 2 mmol/L ammonium acetate solution, and mix well: 5:4 Preparation of standard solution 5:4:1 Chlorpromazine standard stock solution (100 μg/mL): Take about 11 mg of chlorpromazine hydrochloride standard, weigh it accurately, add an appropriate amount of methanol to dissolve and dilute to a 100 mL volumetric flask, shake well, and you get : Store in the dark below -18℃, valid for 6 months: 5:4:2 Internal standard stock solution (100 μg/mL): Take about 11 mg of chlorpromazine hydrochloride-D6 standard, weigh it accurately, add an appropriate amount of methanol to dissolve and dilute to a 100 mL volumetric flask, shake well, and you get : Store in the dark below -18℃, valid for 6 months: 5:4:3 Chlorpromazine standard intermediate solution (500ng/mL): Accurately measure an appropriate amount of chlorpromazine standard stock solution and dilute it with methanol to make a concentration of 500ng/mL chlorpromazine standard intermediate solution: Store in a dark place below -18°C and is valid for 3 months: 5:4:4 Internal standard working solution (200ng/mL): Accurately measure an appropriate amount of the internal standard stock solution, dilute it with methanol to prepare a chlorpromazine-D6 internal standard working solution with a concentration of:200ng/mL: Store in the dark below -18°C ,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: 0:22μm:6 Instruments and equipment6:1 Liquid chromatography-tandem mass spectrometer: equipped with electrospray ion source: 6:2 Balance: sensitivity 0:01g and 0:00001g: 6:3 Homogenizer: 6:4 Centrifuge: 6000r/min: 6:5 Rotary evaporator: 6:6 Vortex mixer: 6:7 Ultrasonic cleaner:7 Measurement steps7:1 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 blank sample after homogenization as the blank sample; c) Take the homogenized blank sample, add the standard intermediate 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 steps8:1 Extraction Take 5g of the sample (accurate to ±0:05g) in a 50mL centrifuge tube, add 50μL of internal standard working solution, add 15mL of acetonitrile, homogenize for 1 minute, and ultrasonic Sonicate for 10 min, centrifuge at 4000 r/min for 7 min, transfer the supernatant to another 50 mL centrifuge tube; take another 10 mL of acetonitrile and clean the homogenizer for 30 s, pour the washing liquid into the residue, vortex and mix for 2 min, ultrasonic for 10 min, 4000 r/min Centrifuge for 7 minutes, combine the supernatant, centrifuge at 6000r/min for 5 minutes, take the supernatant and set aside: 8:2 Purification Take the solid phase extraction column, activate it with 5 mL each of methanol and water, pass the supernatant through the column at a speed of about 1 drop per second, and elute with 5 mL of methanol: Discard the effluent and drain it: Elute with 3 mL of 5% ammoniated methanol solution: Collect the eluate and blow dry with nitrogen at 40°C: Add 30% methanol-ethyl alcohol accurately: Dissolve the residue in 1 mL of ammonium acid solution and filter it with an aqueous needle filter into an injection vial for liquid chromatography-tandem mass spectrometry measurement: 8:3 Preparation of matrix standard curve Accurately measure appropriate amounts of 500ng/mL chlorpromazine standard intermediate solution and:200ng/mL internal standard working solution, blow dry with nitrogen at 40°C, and use blank matrix The solution was prepared into a series of matrices with an isotope internal standard concentration of 10ng/mL and chlorpromazine concentrations of 2:5ng/mL, 5:0ng/mL, 25:0ng/mL, 100:0ng/mL and 250:0ng/mL: The standard working solution is used for liquid chromatography-tandem mass spectrometry: The standard curve is drawn using the ratio of the characteristic ion mass chromatographic peak area of chlorpromazine to the characteristic ion mass chromatographic peak area of the isotope internal standard as the ordinate and the corresponding concentration as the abscissa: Regression equation and correlation coefficient: 8:4 Determination 8:4:1 Liquid chromatography conditions a) Chromatographic column: C18 column, 150mm×2:1mm, 5μm, or equivalent performance; b) Flow rate: 0:2mL/min; c) Column temperature: 25℃; d) Injection volume: 25μL; e) Mobile phase: A is methanol, B is 2mmol/L ammonium acetate, and the gradient elution conditions are shown in Table 1: 8:4:2 Mass spectrometry conditions a) Ion source: electrospray ion source; b) Scanning method: positive ion scanning; c) Detection method: multiple reaction monitoring; d) Spray voltage: 4500V; e) Ion transmission capillary temperature: 300℃; f) In-source collision-induced dissociation voltage: 8V; g) Atomizing gas flow rate: 12:3L/h; h) Auxiliary air flow rate: 1:7L/h; i) The reference values of precursor ions, product ions and collision energy are shown in Table 2: 8:4:3 Determination method Inject equal volumes of sample solution and matrix standard working solution, perform single-point or multi-point calibration, and calculate using the chromatographic peak area and internal standard method: The response values of chlorpromazine in the matrix standard solution and the sample solution should be within the linear range of the instrument detection: The retention time and relative abundance of characteristic ions are compared qualitatively with the retention time and relative abundance of characteristic ions of a matrix standard solution of similar concentration: The retention time deviation of the analyte in the sample solution and the standard substance is within ±2:5%; the relative abundance deviation of the characteristic ions meets the requirements of Table 3, then It can be determined that the corresponding analyte exists in the sample: Under the above chromatography-mass spectrometry conditions, the characteristic ion chromatograms of chlorpromazine and internal standard standard solution See Appendix 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 results10 Method sensitivity, accuracy and precision 10:1 Sensitivity The detection limit of this method is 0:5 μg/kg, and the quantitation limit is 1:0 μg/kg: 10:2 Accuracy In this method, when chlorpromazine is added at a concentration range of 1 μg/kg to 50 μg/kg, the recovery rate is 70% to 110%: 10:3 Precision The intra-batch relative standard deviation of this method is ≤15%, and the inter-batch relative standard deviation is ≤15%: ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 31656.4-2021_English be delivered?Answer: Upon your order, we will start to translate GB 31656.4-2021_English as soon as possible, and keep you informed of the progress. 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