PMID- 33517972 OWN - NLM STAT- MEDLINE DCOM- 20210202 LR - 20210202 IS - 1000-8020 (Print) IS - 1000-8020 (Linking) VI - 50 IP - 1 DP - 2021 Jan TI - [Determination of domoic acid in shellfish by liquid chromatography- tandem mass spectrometry coupled with dispersive solid phase extraction]. PG - 116-142 LID - 10.19813/j.cnki.weishengyanjiu.2021.01.020 [doi] AB - OBJECTIVE: A method utilizing liquid chromatography-tandem mass spectrometry(LC-MS/MS) coupled with dispersive solid phase extraction for quantitative analysis of domoic acid in four kinds of shellfish was established. METHODS: The sample of 0. 1 g was extracted with 25% methanol aqueous solution, the extract was purified by dispersive solid phase extraction with 50 mg HLB and 5 mg GCB, and then filtered through a PTFE membrane. The analytes were separated on a C_(18) column(100 mmx2. 1 mm, 1. 9 mum), and detected in selected reaction monitoring(SRM) mode via positive electrospray ionization. The matrix matching and external standard method was used for quantitation. RESULTS: Domoic acid showed good linearity in the concentration range between 1. 0 ng/mL and 50. 0 ng/mL with correlation coefficients higher than 0. 9994. The detection limits of domoic acid in shellfish was 5 mug/kg. The inter-and intra-day recoveries were 91. 6%-109. 2% and 90. 9%-109. 3%, respectively. The inter-and intra-day ralitive standard deviations(RSDs) were lower than 8. 2% at spiked concentrations of 20, 50 and 100 mug/kg. CONCLUSION: The method is accurate, fast, easy to operate, which can satisfy the requirements of public health emergency testing or routine testing. FAU - Fang, Li AU - Fang L AD - Key Laboratory of Health Risk Factors for Seafood of Zhejiang Province, Zhoushan Municipal Center for Disease Control and Prevention, Zhoushan 316021, China. FAU - Wu, Fan AU - Wu F AD - Wannan Medical College, School of Laboratory Medicine, Wuhu 241002, China. FAU - Qiu, Fengmei AU - Qiu F AD - Daishan Center for Disease Control and Prevention, Zhoushan 316200, China. FAU - Yu, Xinwei AU - Yu X AD - Key Laboratory of Health Risk Factors for Seafood of Zhejiang Province, Zhoushan Municipal Center for Disease Control and Prevention, Zhoushan 316021, China. FAU - Zhu, Yanhua AU - Zhu Y AD - School of Food and Pharmacy, Zhejiang Ocean University, Zhoushan 316022, China. LA - chi PT - Journal Article PL - China TA - Wei Sheng Yan Jiu JT - Wei sheng yan jiu = Journal of hygiene research JID - 9426367 RN - M02525818H (domoic acid) RN - SIV03811UC (Kainic Acid) SB - IM MH - Chromatography, High Pressure Liquid MH - Chromatography, Liquid MH - Kainic Acid/analogs & derivatives MH - Shellfish/analysis MH - *Solid Phase Extraction MH - *Tandem Mass Spectrometry OTO - NOTNLM OT - amnesic shellfish poisoning OT - dispersive solid phase extraction OT - domoic acid OT - liquid chromatography-tandem mass spectrometry OT - shellfish EDAT- 2021/02/02 06:00 MHDA- 2021/02/03 06:00 CRDT- 2021/02/01 05:30 PHST- 2021/02/01 05:30 [entrez] PHST- 2021/02/02 06:00 [pubmed] PHST- 2021/02/03 06:00 [medline] AID - 10.19813/j.cnki.weishengyanjiu.2021.01.020 [doi] PST - ppublish SO - Wei Sheng Yan Jiu. 2021 Jan;50(1):116-142. doi: 10.19813/j.cnki.weishengyanjiu.2021.01.020.