超高效液相色谱-串联质谱法测定水产品中22种邻苯二甲酸酯类环境激素  

Detection of 22 Phthalic Acid Esters(PAEs) of Environmental Hormone in Aquatic Products with High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：方道赠[1] 王宁[1] 张亮 李娜 隋玉杰[1] FANG Daozeng;WANG Ning;ZHANG Liang;LI Na;SUI Yujie(Wenzhou Quality and Technical Supervision Testing Institute,Wenzhou,Zhejiang 325000,China)

机构地区：[1]温州市质量技术监督检测院,浙江温州325000

出　　处：《农产品加工（下）》2018年第10期46-49,共4页Farm Products Processing

基　　金：温州市科技计划项目(2016N0017)

摘　　要：建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)对水产品中22种邻苯二甲酸酯类环境激素同时进行测定的方法。样品经正己烷均质提取,并采用Si/PSA SPE型固相萃取柱净化后进行UPLC-MS/MS仪器分析。提取净化后的溶液经超高效液相色谱柱ZORBAX Eclipse Plus C18(2.1 mm×50 mm,1.8μm)分离后,用甲醇和水(均含0.1%甲酸和5 mmol/L乙酸铵)进行梯度洗脱,所得色谱图表明,22种环境激素均得到有效分离和检测。22种环境激素在10～1 000μg/L质量浓度范围内线性相关系数R2均不低于0.996 8,线性关系良好。回收率在83.5%～103.1%,精密度为2.1%～8.2%。该方法回收率高、重复性好,可用于水产品中邻苯二甲酸酯类环境激素的检测。A method for detction of 22 phthalic acid esters （PAEs） of environmental hormone in aquatic products was developed by using high periormance liquid ctlromatography-tandem mass spectrometry （UPLC-MS/MS） . The samples were extracted with n-hexane and purificated with Si/PSA SPE glass cartridge, and then UPLC-MS/MS analysis was carried out. 22 PAEs were seperated and detected successfully by ZORBAX Eclipse Plus C18 （2.1 mm× 50 mm, 1.8 μm） column seperation with methanol and water, containing 0.1% tomic acid and 5 mmol/L ammonium acetate, as gradient elution solutions. The linear correlation coefficient R2 was not less than 0.996 8 for each PAE in the concentration range of 10~1 000 μg/L, showing good linear relationship. The recovely rates range from 83.5%~103.1% and the RSDs range from 2.1%~8.2%. The method was proved to be suitable for detection of PAEs of environmental hormone in aquatic products.

关 键 词：超高效液相色谱-串联质谱法 水产品 邻苯二甲酸酯 环境激素 

分 类 号：O657.6[理学—分析化学]