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

ABSTRACT

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%.