同位素内标-气相色谱三重四级杆质谱法测定鱼贝类中7种指示性多氯联苯  

Determination of 7 indicative polychlorinated biphenyls in fish ands hellfish by isotope internal standard-gas chromatography-tripleq uadruple mass spectrometry

作　　者：陈柯星[1] 肖明发[1] 林捷[1] 陈华峰[2] 林侃[1] CHEN Ke-xing;XIAO Ming-fa;LIN Jie;CHEN Hua-feng;LIN Kan(Clinical Laboratory,Fuzhou Center for Disease Control and Prevention,Fuzhou,Fujian 350200,China)

机构地区：[1]福州市疾病预防控制中心检验科,福建福州350200 [2]福建省疾病预防控制中心

出　　处：《中国卫生工程学》2024年第5期602-606,共5页Chinese Journal of Public Health Engineering

摘　　要：目的建立鱼贝类中7种指示性多氯联苯(PCBs)的气相色谱-三重四极杆质谱(GC-MS/MS)测定方法。方法将匀浆的鱼贝类样品用无水Na2SO_(4)脱水,正己烷+二氯甲烷(2∶1)超声提取,提取液经酸化硅胶分散固相萃取(DSPE),碱性氧化铝固相萃取小柱净化、浓缩。以DB-XLB色谱柱分离,运用多反应监测扫描模式(MRM)进行扫描测定,同位素内标法定量。结果本方法条件下,7种指示性多氯联苯在0.5~20.0μg/L浓度范围内具有良好的线性关系(r>0.999),以取样2.0 g计,方法的检出限可达到0.010μg/kg。用空白样品进行3个水平加标回收实验(0.6、10.0、18.0μg/L),平均回收率86.1%~104.1%,相对标准偏差(RSD,n=6)0.30%~5.59%。结论本方法操作简便,定量准确可靠,适用于鱼贝类样品中7种指示性多氯联苯的测定。Objective To establish a gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method for the determination of 7 indicative polychlorinated biphenyls(PCBs)in fish and shellfish.Methods Homogenized fish and shellfish samples were dehydrated with anhydrous Na_2SO_4,PCBs were ultrasonically extracted with n-hexane+dichloromethane(2∶1),and the extract was purified by acidified silica gel dispersion solid phase extraction(DSPE)and alkaline alumina solid phase extraction column.After concentration,the target analytes were separated on DB-XLB chromatographic column,analyzed by GC-MS/MS under multiple reaction monitoring(MRM)scanning mode,and quantified by isotope internal standard method.Results In this method,the calibration curves for all target analytes showed good linearity in the range of 0.5-20.0μg/L(r>0.999),the limit of determination was 0.010μg/kg by sampling 2 g.The average recoveries of the 7 indicative PCBs were from 86.1%to 104.1%at three spiked levels of 0.60,10.0 and 18.0μg/L,and the relative standard deviations(RSD,n=6)was from 0.30%to 5.59%.Conclusion The method is simple,accurate,reliable,and suitable for the determination of 7 indicative PCBs in fish and shellfish samples.

关 键 词：指示性多氯联苯 气相色谱-三重四极杆质谱 同位素内标法 鱼贝类 

分 类 号：O657.63[理学—分析化学] R155.5[理学—化学]