水产品中五氯酚及其钠盐的高效液相色谱串联质谱检测方法的优化  

Research on an optimized liquid chromatography-tandem mass spectrometry method for the determination of pentachlorophenol and its sodium salts in aquatic products

作　　者：李诗言[1] 王鼎南 周凡[1] 柯庆青 贝亦江[1] 吴洪喜[1] 丁雪燕[1] 王扬[1] LI Shiyan;WANG Dingnan;ZHOU Fan;KE Qingqing;BEI Yijiang;WU Hongxi;DING Xueyan;WANG Yang(Aquatic Products Quality Inspection Center of Zhejiang Province,Hangzhou 310023,China)

机构地区：[1]浙江省水产质量检测中心

出　　处：《中国渔业质量与标准》2019年第5期23-29,共7页Chinese Fishery Quality and Standards

基　　金：国家特色淡水鱼产业技术体系(CARS-46);浙江省“十三五”水产新品种选育重大科技专项——南美白对虾(2016C02055-5-2)

摘　　要：对水产品中五氯酚及其钠盐的高效液相色谱串联质谱检测方法进行了深入优化。样品通过三乙胺碱化的70%乙腈水溶液提取,使目标物保持在离子态,之后采用大粒径的阴离子交换(MAXLP)小柱进行富集,依次用5%氨水(V/V)溶液、甲醇和50%的甲醇水溶液(含2%甲酸,V/V)进行淋洗,最后用5mL的4%甲酸甲醇溶液洗脱。净化浓缩后样品采用C18色谱柱进行分离,以甲醇和5mmol/L乙酸铵水溶液为流动相进行梯度洗脱,多反应监测负离子模式扫描,采用同位素稀释内标法定量。目标化合物在相关范围内线性关系良好,相关系数r不低于0.99,方法在不同水产品基质中的定量限均为0.5μg/kg,基质加标回收率范围为92.4%~102.0%,相对标准偏差为3.21%~9.15%。经验证,本研究优化后的方法适用于水产品中五氯酚及其钠盐的残留检测,且相比标准方法,减少了前处理所需时间,同时避免了堵柱情况出现,解决了蟹类样品回收率偏低的问题。An optimized method for the simultaneous and rapid determination of pentachlorophenol and its sodium salt in aquatic products was developed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were firstly extracted with 70% acetonitrile-water (5% triethylamine, V/V ), and then enriched and cleaned up using a large particle size MAX LP SPE column by 5% ammonia solution, methanol and 50% methanol solution (2% formic acid, V/V ) as leacheates. Finally, the target compounds were eluted with 5 mL of 4% formic acid methanol solution. The samples were analyzed directly on a C 18 column using 5 mmol/L ammonium acetate and methanol as mobile phase. The quantitative determination of the analytes was carried out under the multiple reaction monitoring mode with negative electrospray ionization. The samples were quantified by the isotope dilution and internal standard methods. The calibration curves were linear well in the corresponding concentration ranges, with correlation coefficient r ≥ 0.99 . The limits of quantification were 0.5 μg/kg. The average spiked recoveries were between 92.4% and 102.0% with the relative standard deviations of 3.21%-9.15%. The proposed method is sensitive, accurate, and efficient for the determination of pentachlorophenol and its sodium salt residues in aquatic products. Compared with the standard method, the proposed method has less pretreatment time, no column blocking situation, and be able to improve the low recovery rate problem for crab samples.

关 键 词：高效液相色谱串联质谱法 五氯苯酚 五氯酚钠 水产品 内标法 定量限 

分 类 号：S94[农业科学—水产养殖]