高效液相色谱质-谱联用法测定西加鱼毒素P-CTX-1  

Determination of ciguatoxin P-CTX-1 by high performance liquid chromatography-mass spectrometry

作　　者：桓清柳[1] 吴霓[1] 王爱辉[1] 温众杰[1] 江天久[1] 

机构地区：[1]暨南大学赤潮与海洋生物学研究中心,广州510632

出　　处：《分析试验室》2013年第7期1-5,共5页Chinese Journal of Analysis Laboratory

基　　金：国家重点基础研究发展规划项目(973)(2010CB428702);国家自然科学基金项目(41276091);NSFC-广东联合基金项目(U0733006);国家赤潮灾害调查专项(908)(SZ801)资助

摘　　要：建立了对西加鱼毒素中主要成分P-CTX-1的高效液相色谱质谱联用检测方法。色谱条件为色谱柱C18(2.1mm×50mm,1.7μm),柱温40℃。以0.1%甲酸-5mmol/L乙酸铵水溶液和乙腈溶液作为流动相,梯度洗脱(0～3.0min50%A→5%A,3.0～4.5min5%A→50%A),流速为0.6mL/min。质谱条件为电喷雾正离子模式,[M+NH4]+作为前体离子进行多级反应监测,以质荷比(m/z)为1058和1076的子离子分别作为P-CTX-1的定性和定量离子,源温度105℃,喷雾温度350℃,提取电压4.0V,锥气流速49mL/min,喷雾气流速750L/h。在此检测条件下西加鱼毒素P-CTX-1的检出限达0.175μg/L,平均加标回收率为66.0±2.0%,相对标准偏差为6.0%。利用该方法检测了6份采自西太平洋珊瑚礁的鱼类样品,在其中5份样品中检测出P-CTX-1。A quantitative method was developed with high performance liquid chromatography-mass spectrometry （LC-MS/MS） to determine ciguatoxin which is mainly focused on P-CTX-1. The analysis of P-CTX-1 was performed on a C18 column （2. 1 mm x 50 mm, 1.7 μm） using gradient elution with 0. 1% formic acid containing 5 mmol/L ammonium acetate and aeetonitrile at 40 ℃. The gradient elution was from 50% to 5% in the first 3.0 min and then back to 50% in the next 1.5 min, at a flow rate of 0. 6 mL/min. Detection was performed in multiple reaction monitoring mode with [ M ＋ NH4 ]＋ as the precursor ion. Fragment ions with m/z 1076 and 1058 were used as qualitative and quantitative ions of P-CTX-1. The source temperature and desolvation temperature were 105℃ and 350 ℃ respectively. The extraction voltage is 4. 0 V. The cone gas flow rate was 49 mL/min and the desolvation gas flow rate was 750 L/h. The result showed that the limit of quantitation was 0. 175μg/L. The average recovery was 66.0 ± 2. 0% with the relative standard deviation （RSD） of 6.0%. Six samples of coral reef fish from western pacific were tested by using the method mentioned above, and P-CTX-1 was found in five samples.

关 键 词：西加鱼毒素 太平洋雪卡毒素 高效液相色谱-质谱联用 检测 

分 类 号：O657.63[理学—分析化学]