PMID- 20712117 OWN - NLM STAT- MEDLINE DCOM- 20120105 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 28 IP - 4 DP - 2010 Apr TI - [Determination of azaspiracid-1 in shellfishes by liquid chromatography with tandem mass spectrometry]. PG - 363-7 AB - A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of azaspiracid-1 (AZA1) in shellfishes was described. After being extracted using methanol and water (80:20, v/v), the extract was cleaned-up by solid phase extraction (SPE) of MAX column, then determined by using a reversed-phase high performance liquid chromatography (HPLC) isocratic program coupled with tandem mass spectrometry in selected reaction monitoring mode (SRM). And the extract was eluted with acetonitrile-water (80:20, v/v) on an Atlantis dC18 column (150 mm x 4.6 mm, 5.0 microm) with mobile phase containing 50 mmol/L formic acid and 2 mmol/L ammonium formate. The detection limit was 11.00 pg/g. The calibration curve was linear (R2 = 0.998 1) in the range of 48.85-2 442 ng/L. The average recoveries of the shellfish tissue extract at three spiked levels (36.64, 73.27, 146.54 pg/g) were from 75.8% to 82.5% (n = 6). The relative standard derivations (RSDs) were less than 10%. The 112 shellfish samples from the local markets of Dalian, Qingdao, Guangzhou were detected by the method, and AZA1 was detected in some samples from Dalian and Guangzhou. The results showed that the method is simple, rapid, sensitive and suitable for the detection of AZA1 in shellfishes. FAU - Yao, Jianhua AU - Yao J AD - Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China. FAU - Tan, Zhijun AU - Tan Z FAU - Zhou, Deqing AU - Zhou D FAU - Guo, Mengmeng AU - Guo M FAU - Xing, Lihong AU - Xing L FAU - Yang, Shouguo AU - Yang S LA - chi PT - English Abstract PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Marine Toxins) RN - 0 (Spiro Compounds) RN - 0 (azaspiracid) SB - IM MH - Animals MH - Bivalvia/chemistry MH - Chromatography, High Pressure Liquid/*methods MH - Marine Toxins/*analysis MH - Sensitivity and Specificity MH - Shellfish/*analysis MH - Spiro Compounds/*analysis MH - Tandem Mass Spectrometry/*methods EDAT- 2010/08/18 06:00 MHDA- 2012/01/06 06:00 CRDT- 2010/08/18 06:00 PHST- 2010/08/18 06:00 [entrez] PHST- 2010/08/18 06:00 [pubmed] PHST- 2012/01/06 06:00 [medline] AID - 10.3724/sp.j.1123.2010.00363 [doi] PST - ppublish SO - Se Pu. 2010 Apr;28(4):363-7. doi: 10.3724/sp.j.1123.2010.00363.