CAJ | 학술논문

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,C_(18)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.
건립료고효액상색보-전분무천련질보법측정어체중설잡독소P-CTX1함량적방법.어류양품경병동제취후,용냉동탈지,경PSA고상췌취주정화후,C_(18)색보주분리,채용전분무천련사겁간질보진행검측.결과표명,설잡독소재0.5～20 μg/L범위시,선성관계량호(r=0.9998).P-CTX1재첨가농도위1.0～20.0 ng/kg범위내적평균회수솔위82.3%～87.2%,상대표준편차소우7.8%,방법적정량검출한위0.1 μg/L.
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%.