Geng Dawei, Jogsten Ingrid Ericson, Dunstan Jody, Hagberg Jessika, Wang Thanh, Ruzzin Jerome, Rabasa-Lhoret Rémi, van Bavel Bert
MTM Research Centre, School of Science and Technology, Örebro University, SE-701 82 Örebro, Sweden.
MTM Research Centre, School of Science and Technology, Örebro University, SE-701 82 Örebro, Sweden.
J Chromatogr A. 2016 Jul 1;1453:88-98. doi: 10.1016/j.chroma.2016.05.030. Epub 2016 May 9.
A method using a novel atmospheric pressure chemical ionization source for coupling gas chromatography (GC/APCI) to triple quadrupole mass spectrometry (MS/MS) for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) regulated by the Stockholm Convention is presented. One microliter injection of a six-point calibration curve of native PCBs and OCPs, ranging from 0.04 to 300pg/μL, was performed. The relative standard deviation (RSD) of the relative response factors (RRFs) was less than 15% with a coefficient of determination (r(2))>0.995. Meanwhile, two calibration solutions (CS), CS 2 (0.4pg/μL) and CS 3 (4pg/μL) were analyzed to study the repeatability calculated for both area and RRFs. The RSD for RRF ranged from 3.1 to 16% and 3.6 to 5.5% for CS 2 and CS 3, respectively. The limits of detection (LOD) determined by peak-to-peak signal-to-noise ratio (S/N) of 3 were compared between the GC/APCI/MS/MS and a GC coupled to high resolution mass spectrometry (GC/HRMS) system. GC/APCI/MS/MS resulted in lower LOD for most of the compounds, except for PCB#74, cis-chlordane and trans-chlordane. GC/APCI/MS/MS and GC/HRMS were also compared by performing analysis on 75 human serum samples together with eight QA/QC serum samples. The comparison between GC/APCI/MS/MS system and GC/HRMS system for 16 of the targeted compounds was carried out. No statistically significant difference was discovered. Due to increased sensitivity and user friendly operation under atmospheric pressure, GC/APCI/MS/MS is a powerful alternative technique that can easily meet the specification of GC/HRMS.
本文介绍了一种使用新型大气压化学电离源将气相色谱（GC/APCI）与三重四极杆质谱（MS/MS）联用的方法，用于测定《斯德哥尔摩公约》管控的有机氯农药（OCPs）和多氯联苯（PCBs）。对浓度范围为0.04至300pg/μL的天然PCBs和OCPs进行六点校准曲线的1微升进样。相对响应因子（RRFs）的相对标准偏差（RSD）小于15%，决定系数（r(2)）>0.995。同时，分析两种校准溶液（CS），即CS 2（0.4pg/μL）和CS 3（4pg/μL），以研究面积和RRFs的重复性。CS 2和CS 3的RRF的RSD分别为3.1%至16%和3.6%至5.5%。比较了GC/APCI/MS/MS和与高分辨率质谱联用的气相色谱（GC/HRMS）系统通过峰峰信噪比（S/N）为3确定的检测限（LOD）。除了PCB#74、顺式氯丹和反式氯丹外，GC/APCI/MS/MS对大多数化合物的LOD较低。还通过对75份人血清样本和8份质量保证/质量控制血清样本进行分析，比较了GC/APCI/MS/MS和GC/HRMS。对16种目标化合物进行了GC/APCI/MS/MS系统和GC/HRMS系统的比较。未发现统计学上的显著差异。由于在大气压下灵敏度提高且操作方便，GC/APCI/MS/MS是一种强大的替代技术，能够轻松满足GC/HRMS的规格要求。
