基质固相分散-气相色谱串联质谱法测定孕妇血清中22种持久性有机污染物

Determination of 22 Kinds of Persistent Organic Pollutants in Serum of Pregnant Women by Matrix Solid Phase Dispersion Procedure and Gas Chromatography Coupled to Triple Quadrupole Mass Spectrometry

建立了基质固相分散技术-气相色谱串联质谱法（MSPD-GC-QQQ-MS/MS）同时测定孕妇血清中22种持久性有机污染物（艾氏剂、狄氏剂、七氯、灭蚁灵、六六六、多氯联苯和滴滴涕）的方法。血清样品与C18吸附剂混合净化,正己烷溶液洗脱,GC-QQQ-MS/MS测定。采用Agilent J＆W DB-35ms（30 m×0.25 mm×0.25μm）分离,正电子离子源（EI＋）模式电离,多反应监测模式（MRM）下进行测定,外标法定量。结果表明,在1.0~1000.0 ng/m L的范围内,22种持久性有机污染物的相关系数均大于0.99;在2.0和20.0 ng/m L的添加水平下,所有持久性有机污染物回收率均在75%~115%之间,方法定量限均≤0.15 ng/m L。在比较基质固相分散（MSPD）、液液萃取（LLE）和固相萃取（SPE）提取和净化实际加标血清样品时,MSPD方法的结果中位数更接近真实值,且离散程度最小。本方法适用于人类血清中多种持久性有机物的定性和定量分析。

A method was developed for the simultaneous determination of 22 kinds of persistent organic pollutants （POPs） （Aldrin, Dieldrin, Mirex, HCHs, DDTs and PCBs） in serum of pregnant women by matrix solid phase dispersion procedure and gas chromatography coupled to triple quadrupole mass spectrometry （MSPD-GC-QQQ-MS/MS）. The serum samples were blended with C18 adsorbent and eluted by n-hexane. Agilent DB-35MS column （30 m×0.25 mm×0.25 μm） was used to separate 22 kinds of POPs with high sensitivity and satisfactory resolution. The identification and quantification were achieved by using electron ionization in positive ion mode （EI＋） with multiple reaction monitoring （MRM）. The results showed that matrix-matched calibration curves with good correlation coefficients （R2〉 0.99 ） were obtained in the concentration range of 1. 0 - 1000. 0 ng/mL. The recoveries of the spiked samples at 2. 0 ng/mL and 20.0 ng/mL were in the range of 75% to 115% with the RSD lower than 13%. The limits of quantification （LOQ） for 22 kinds of POPs were ≤0.15 ng/mL. Liquid-liquid extraction （LLE） and solid phase extraction （SPE） were used to compare with the MSPD method by spiked serum and the efficiency of the methods mentioned above was evaluated by determining the concentration of POPs （ng/mg lipid）. Median value obtained by MSPD method was the closest to actual concentration, and the dispersion of all data was minimal. The method was successfully applied to the simultaneous determination of POPs for quantification and confirmation in human serum.