Determination of azaspiracid-1 in shellfishes by liquid chromatography with tandem mass spectrometry

被引:37
|
作者
Yao Jianhua [1 ,2 ]
Tan Zhijun [1 ]
Zhou Deqing [1 ]
Guo Mengmeng [1 ]
Xing Lihong [1 ]
Yang Shouguo [1 ,2 ]
机构
[1] Chinese Acad Fishery Sci, Yellow Sea Fisheries Res Inst, Qingdao 266071, Peoples R China
[2] Shanghai Ocean Univ, Coll Food Sci & Technol, Shanghai 201306, Peoples R China
关键词
liquid chromatography with tandem mass spectrometry (LC-MS/MS); shellfish poisoning; azaspiracid; shellfish;
D O I
10.3724/SP.J.1123.2010.00363
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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 dC(18) column (150 mm x 4.6mm, 5.0 mu m) 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 (R-2 = 0.9981) in the range of 48.85 - 2442 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.
引用
收藏
页码:363 / 367
页数:5
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