摘要
目的建立饮用水中20种多氯联苯(PCBs)的液液微萃取-气相色谱-三重四极杆质谱联用(GC-MS/MS)测定方法。方法采用液液微萃取富集,离心分离,13C内标法定量。采用EI源,在多反应监测(MRM)模式下进行检测。结果 20种PCBs在5.0 ng/L^200 ng/L(高氯联苯20.0 ng/L^200.0 ng/L)时,线性关系良好,相关系数(r)为0.997 5~0.999 7,方法的检出限为0.35 ng/L^6.60 ng/L,定量限为1.04 ng/L^19.7ng/L。在0.020μg/L和0.10μg/L 2种水平下的加标回收率为78.2%~114.0%,相对标准偏差为4.6%~10.5%。方法的富集倍数为301倍~632倍。结论本方法采用液液微萃取前处理,气相色谱-三重四级杆质谱联用法多反应监测,水样处理简单、快速、可靠。通过应用7种13C同位素内标物,减少了基质干扰,使目标物得到较好的分离。用GC-MS/MS检测特征离子的二级离子,提高了灵敏度,增强了定性、定量的准确度。可用于生活饮用水中20种PCBs的测定。
Objective To develop a method for the determination of polychlorinated biphenyls（PCBs） in drinking water by gas chromatography - triple quadrupole mass spectrometry after liquid - liquid microextraction. Methods PCBs in water sample were extracted and enriched by liquid - liquid mieroextration for centrifugal separation, with i3C internal standard method for quantification; and then determined in multiple reaction monitoring（MRM） mode with EI source. Results The method showed good linearity when the concentration of 20 PCBs were within 5.0 ng/L - 200.0 ng/L（ High chlorine was within 20.0 ng/L - 200.0 ng/L）, with the correlation coefficient（r） within 0. 997 5 -0. 999 7. The limits of detection were within 0.35 ng/L - 6.60 ng/L. The limits of quantification were 1.04 ng/L - 19.7 ng/L. The average recovery was within 78.2% - 114.0% at the spiked levels of 0. 020 μg/L and 0.10 μg/L. The relative standard derivations were within 4.6% - 10.5%. The enrich- ment factors were within 301 time - 632 time. Conclusion The method for determination of PCBs in drinking water by gas chromatography - triple quadrupole mass spectrometry after liquid - liquid microextraction was rapid, simple and reliable, which used 7 13C PCBs as internal standards to reduce the background interference. The PCBs were effective separated. The secondary characteristic ions were used to improve the sensitivity and accuracy. It is suitable for determination of 20 PCBs in drinking water.
出处
《中国卫生检验杂志》
CAS
2016年第14期2006-2008,2012,共4页
Chinese Journal of Health Laboratory Technology
关键词
多氯联苯
气相色谱-三重四级杆质谱联用法
液液微萃取
生活饮用水
Polychlorinated biphenyls
Gas chromatography triple quadrupole mass spectrometry
Liquid -liquid microextrac-tion
Drinking water
