Fang Jing, Wu Qian, Zhao Yun, Zhao Hongzhi, Xu Shunqing, Cai Zongwei
State Key Laboratory of Environmental and Biological Analysis, Department of Chemistry, Hong Kong Baptist University, Hong Kong SAR, China.
Key Laboratory of Environment and Health (Huazhong University of Science and Technology), Ministry of Education & Ministry of Environmental Protection, and State Key Laboratory of Environmental Health (Incubation), School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430030, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Jan 1;1040:180-185. doi: 10.1016/j.jchromb.2016.12.001. Epub 2016 Dec 5.
Gas chromatography-triple quadrupole mass spectrometry (GC-QqQMS) was applied for the determination of eight organochlorine pesticides (OCPs) in human serum. OCPs were extracted from the serum sample by solid phase extraction (SPE) and analyzed by gas chromatography mass spectrometry (GC-MS) or gas chromatography tandem mass spectrometry (GC-MS/MS). Electron ionization (EI) and negative chemical ionization (NCI) under two data acquisition modes, namely selected ion monitoring (SIM) and multiple reaction monitoring (MRM), were compared. The use of MRM generally provided higher selectivity and sensitivity because less interference from the sample matrix existed. The EI mode is more suitable for less electronegative compounds such as dichlorodiphenyldichloroethanes (DDDs) with detection limits ranging from 0.0060 to 0.060ng/mL. In the NCI mode, MRM analysis provided good and lower detection limits (0.0011-0.0030ng/mL) for pesticides containing more chlorines. The methods were validated by analyzing the pesticides in spiked serum at different levels with recoveries ranged from 83% to 116% and relative standard deviations of less than 10%. The developed method was applied for the determination of the OCPs in real human serum samples.
采用气相色谱 - 三重四极杆质谱联用仪（GC - QqQMS）测定人血清中的8种有机氯农药（OCPs）。通过固相萃取（SPE）从血清样品中提取OCPs，并用气相色谱质谱联用仪（GC - MS）或气相色谱串联质谱仪（GC - MS/MS）进行分析。比较了在两种数据采集模式下，即选择离子监测（SIM）和多反应监测（MRM）时的电子电离（EI）和负化学电离（NCI）。由于来自样品基质的干扰较少，MRM的使用通常提供更高的选择性和灵敏度。EI模式更适合于电负性较小的化合物，如二氯二苯二氯乙烷（DDDs），其检测限为0.0060至0.060ng/mL。在NCI模式下，MRM分析为含氯量较高的农药提供了良好且较低的检测限（0.0011 - 0.0030ng/mL）。通过分析不同加标水平血清中的农药对方法进行验证，回收率在83%至116%之间，相对标准偏差小于10%。所建立的方法应用于实际人血清样品中OCPs的测定。
