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HYT0319-2021: Shellfish - Determination of lipophilic marine biotoxins - LC-MS/MS method
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Shellfish - Determination of lipophilic marine biotoxins - LC-MS/MS method
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HY/T 0319-2021
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Standard similar to HYT0319-2021 HJ 491 GB/T 17136 HY/T 216 Basic data | Standard ID | HY/T 0319-2021 (HY/T0319-2021) | | Description (Translated English) | Shellfish - Determination of lipophilic marine biotoxins - LC-MS/MS method | | Sector / Industry | Marine Industry Standard (Recommended) | | Classification of Chinese Standard | Z19 | | Word Count Estimation | 14,129 | | Issuing agency(ies) | Ministry of Natural Resources of the People's Republic of China | HYT0319-2021: Shellfish - Determination of lipophilic marine biotoxins - LC-MS/MS 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.
Shellfish - Determination of lipophilic marine biotoxins - LC-MS/MS method
ICS 07.060;13.020
CCSZ19
Marine Industry Standard of the People's Republic of China
Detection of Lipid-soluble Marine Biological Toxins in Shellfish
Liquid chromatography-tandem mass spectrometry
LC-MS/MSmethod
Released on 2021-07-02
2021-11-01 implementation
Issued by the Ministry of Natural Resources of the People's Republic of China
Table of contents
Foreword Ⅰ
1 Scope 1
2 Normative references 1
3 Principle 1
4 Reagents and materials 1
5 Equipment 2
6 Sample 3
7 Test Step 3
8 Calculation and expression of results 5
9 Precision 6
10 other 6
Appendix A (informative) Fat-soluble marine biological toxins 7
Appendix B (informative) Characteristic ion mass chromatogram 8
Appendix C (Normative) Toxicity factor 10 of fat-soluble marine biological toxins
Reference 11
Foreword
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules of Standardization Documents"
Drafting.
This document was proposed by the Ministry of Natural Resources of the People's Republic of China.
This document is under the jurisdiction of the National Marine Standardization Technical Committee (SAC/TC283).
Drafting organizations of this document. National Marine Environmental Monitoring Center, Institute of Oceanology, Chinese Academy of Sciences, Xiamen University, Chinese Academy of Fishery Sciences
Yellow Sea Research Institute.
The main drafters of this document. Xu Daoyan, Liang Yubo, Liu Renyan, Liu Lei, Chen Meng, Yu Rencheng, Tan Zhijun, Gao Chunlei, Xu Yanlong.
Detection of Lipid-soluble Marine Biological Toxins in Shellfish
Liquid chromatography-tandem mass spectrometry
Warning---In order to avoid the harm of toxins, please wear gloves for operation. Used equipment such as pipettes and pipette tips, and discarded extraction
The liquid should be soaked in sodium hypochlorite solution (5%) for more than 1 hour to decompose toxins.
1 Scope
This document specifies the shellfish fat-soluble marine biological toxins Daejeon, Dinophyton, Saxitoxin, Ezo scallop toxin, Protodin
Principles, operating procedures and result calculations of 11 toxin compounds such as acid toxins and cyclic imine toxins by liquid chromatography-tandem mass spectrometry.
This document is applicable to the detection of fat-soluble marine biological toxins in shellfish bodies.
2 Normative references
The content of the following documents constitutes an indispensable clause of this document through normative references in the text. Among them, dated quotations
Only the version corresponding to the date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to
This document.
GB/T 6682 Analyze laboratory water specifications and test methods.
3 Principle
Shellfish samples are extracted with methanol, hydrolyzed under alkaline conditions to release the esterified biological toxins, and purified with HLB solid-phase extraction column.
Chromatographic separation, tandem mass spectrometry determination, external standard curve method quantification.
4 Reagents and materials
4.1 Acetonitrile (CH3CN). chromatographically pure.
4.2 Methanol (CH3OH). chromatographically pure.
4.3 Formic acid (HCOOH).
4.4 Ammonium formate (HCOONH4).
4.5 Ammonia (NH3·H2O). concentration ≥ 25%.
4.6 Sodium hydroxide (NaOH).
4.7 Hydrochloric acid (HCL). concentration ≥36%.
4.8 Sodium hydroxide solution (2.5mol/L). accurately weigh 50g of sodium hydroxide, dilute to 500mL with water, and store at room temperature.
4.9 Hydrochloric acid solution (2.5mol/L). accurately measure 104.5mL of hydrochloric acid, dilute to 500mL with water, and store at room temperature.
4.10 Methanol solution (30%). Measure 30mL of methanol and add it to 70mL of water, mix well, at room temperature, and use it now.
4.11 Methanol solution (20%). Measure 20mL of methanol and add it to 80mL of water, mix well, at room temperature, and use it now.
4.12 Ammonia methanol solution (0.3%). Draw 0.3mL ammonia, dilute to 100mL with methanol, at room temperature, and use it now.
4.13 Fat-soluble marine biotoxin standards (see Appendix A) solutions. OA, DTX1, DTX2, PTX2, YTX, homoYTX, AZA1,
The purity of AZA2, AZA3, GYM, SPX1 standard materials is ≥97%, and it should be stored at -20℃ in the dark.
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