高效液相色谱-电喷雾串联质谱法测定鱼体中雪卡毒素

建立了高效液相色谱-电喷雾串联质谱法测定鱼体中雪卡毒素P-CTX1含量的方法.鱼类样品经丙酮提取后,用冷冻脱脂,经PSA固相萃取柱净化后, C18色谱柱分离,采用电喷雾串联四极杆质谱进行检测.结果表明,雪卡毒素在0.5～20 μg/L范围时,线性关系良好(r=0.9998).P-CTX1在添加浓度为1.0～20.0 ng/kg范围内的平均回收率为82.3%～87.2%, 相对标准偏差小于7.8%,方法的定量检出限为0.1 μg/L.

High Performance Liquid Chromatography Coupled with Electrospray Tandem Mass Spectrometry for Analysis of Pacific Ciguatoxin in Fishes

A sensitive method was developed for the determination of pacific ciguatoxin (P-CTX1) residue in fishes by high performance liquid chromatography coupled with electrospray tandem mass spectrometry ( HPLC-MS/MS). Homogenized samples of fish was extracted with acetone,degreased by freezing under -20℃ and filtered with filter paper. Then the supernatant was cleaned up with PSA column. Identification was achieved by electrospray ionization (ESI) in positive mode using multiple reaction monitoring. The calibration curve of P-CTX1 showed good linearity in the range of 0.5 -20μg/L with correlation coefficient of 0.9998. The limit of quantitation (LOQ) was 0. 1 mg/L( S/N = 10). The recoveries of P-CTX1 were between 82. 3% and 87. 2% (n =7) at spiked levels of 1.0 -20.0 ng/kg. The relative standard derivations( RSD) of the method were less than 7.8%.