气相色谱/质谱法检测小鼠肌肉组织和血液中羟基多氯联苯

Determination of Hydroxylated Polychlorinated Biphenyls in Mouse Tissues and Blood by Gas Chromatography/Mass Spectrometry

建立了测定小鼠肌肉和血液中3种羟基多氯联苯的气相色谱/质谱联用(GC-MS)方法。经正己烷-乙酸乙酯(1∶1,V/V)提取目标化合物后,结合H2SO4去脂,KOH反萃法对提取液进行净化,以双(三甲基硅烷基)三氟乙酰胺-三甲基氯硅烷(BSTFA-TMCS,99∶1,V/V,)为衍生试剂对羟基多氯联苯进行硅烷化衍生后,在SIM模式下进行GC/MS分析。本方法检出限为2μg/kg。在3种添加水平2.0,5.0和20.0μg/kg下,小鼠肌肉和血液中3种羟基多氯联苯的回收率范围为73.2%～113.2%;相对标准偏差为1.53%～10.4%。本方法可用于小鼠腹腔注射多氯联苯后,体内多氯联苯羟基代谢物的检测。

A method has been established to determine three hydroxylated metabolites of polychlorinated biphenyls（PCBs） in mouse muscle and blood by GC /MS.Target compouds were extracted by using hexaneethyl acetate as extracting solvents（1：1,V/V）.To obtain satisfactory peak shape and separation efficiency,sulfuric acid and alkaline stripping solution were used to remove the impurities.Derivatizing reagent was N,O-bis（trimethylsilyl）-trimethylchlorosilane（BSTFA-TMCS,99：1,V/V）.The target compounds were analyzed by GC/MS under SIM mode after silylation derivtization.The average recoveries of 3-hydroxy-2,2＇,4＇,5,5＇-PeCB,4-hydroxy-2＇,3,3＇,4＇,5＇-PeCB and 4-hydroxy-2＇,3,3＇,5＇,6＇-PeCB ranged from 73.2% to 113.2 % spiked at 3 levels of 2,5,20μg/kg in muscle and blood.The range of relative standard deviations（RSD） in spiked samples was 1.5%-10.4%.And the detection limit of the method was 2 μg/kg.This established method has been successfully applied to the determination of hydroxylated metabolite in mouse tissues after intraperitoneal injection of 2,2＇,4＇,5,5＇-PeCB at the dose of 10 mg/kg.