气相色谱-串联质谱法测定PM2.5中7种指示性多氯联苯和16种多环芳烃
GC-MS/MS Determination of 7 Indicative Polychlorinated Biphenyls and 16 Polycyclic Aromatic Hydrocarbonds in PM2.5
摘 要
采集PM2.5样品后的滤膜经正己烷与二氯甲烷以体积比1：1组成的混合液超声提取3次，合并提取液，浓缩后用水定容至5.0 mL，采用气相色谱-串联质谱法测定样品溶液中7种指示性多氯联苯和16种多环芳烃的含量。在气相色谱分离中采用DB-5MS UI色谱柱，在串联质谱分析中采用多反应监测模式。7种指示性多氯联苯和16种多环芳烃的质量浓度均在5~200 μg·L-1内与其对应的峰面积呈线性关系，检出限（3S/N）为0.002~0.019 ng·m-3。 以空白样品为基体进行加标回收试验，所得回收率为80.4%~108%，测定值的相对标准偏差（n=6）为0.90%~5.0%。
指示性多氯联苯
多环芳烃
PM2.5
GC-MS/MS
indicative polychlorinated biphenyl
polycyclic aromatic hydrocarbond
PM2.5
Abstract
After sampling PM2.5, the filter membrane was extracted 3 times ultrasonically with the mixture of n-hexane and dichloromethane (volume ratio of 1∶1). The combined extract was concentrated, and then diluted to 5.0 mL with water. GC-MS/MS was applied to the determination of 7 indicative polychlorinated biphenyls and 16 polycyclic aromatic hydrocarbonds in the sample solution. The DB-5MS UI chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination. Linear relationships between values of peak area and mass concentration of 7 indicative polychlorinated biphenyls and 16 polycyclic aromatic hydrocarbonds were kept in the same range of 5-200 μg·L-1, with detection limits (3S/N) in the range of 0.002-0.019 ng·m-3. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 80.4%-108%, with RSDs (n=6) of determined values in the range of 0.90%-5.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202012003
所属栏目 试验与研究
基金项目 国家重大公共卫生项目（001002034023）；辽宁省科技重点实验室项目（2017）
收稿日期 2020/4/29
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备注曹忠波,副主任技师,主要从事理化分析检验工作
引用该论文: CAO Zhongbo,ZHANG Yuanyuan,LIU Xiaojing,CHEN Xi,HUA Zhenggang. GC-MS/MS Determination of 7 Indicative Polychlorinated Biphenyls and 16 Polycyclic Aromatic Hydrocarbonds in PM2.5[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(12): 1261～1266
曹忠波,张媛媛,刘晓晶,陈曦,华正罡. 气相色谱-串联质谱法测定PM2.5中7种指示性多氯联苯和16种多环芳烃[J]. 理化检验－化学分册, 2020, 56(12): 1261～1266
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参考文献
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【14】马英歌,孙谦,景盛翱,等.超声萃取结合气相色谱三重四极杆质谱联用法测定PM2.5大气污染物中多环芳烃含量[J].环境化学, 2015,34(12):2327-2329.
【2】ZACS D, RJABOVA J, VIKSNA A, et al. Method development for the simultaneous determination of polybrominated, polychlorinated, mixed polybrominated/chlorinated dibenzo-p-dioxins and dibenzofurans, polychlorinated biphenyls and polybrominated diphenyl ethers in fish[J]. Chemosphere, 2015,118:72-80.
【3】陶永进,曾娅莉,邓建军,等.PM2.5沙尘矿物的6种主要成分致A549细胞遗传毒性研究[J].工业卫生与职业病, 2016,42(5):321-325.
【4】黄强,董发勤,王利民,等.PM2.5中的矿物粉尘对V79细胞毒性研究[J].工业卫生与职业病, 2015,41(2):81-85.
【5】HELMFRID I, SALIHOVIC S, VAN BAVEL B, et al. Exposure and body burden of polychlorinated biphenyls (PCB) and metals in a historically contaminated community[J]. Environment International, 2015,76:41-48.
【6】齐丽,李楠,任玥,等.北京地区典型二噁英(PCDDs)及多氯联苯(PCBs)的长距离传输潜力——基于TaPL3模型的应用研究[J].环境化学, 2013,32(7):1149-1157.
【7】LÓPEZ CANCIO J A, CASTELLANO A V, MARTÍN S S, et al. Size distributions of PAHs in ambient air particles of two areas of Las palmas de gran Canaria[J]. Water, Air, & Soil Pollution, 2004,154(1/2/3/4):127-138.
【8】田福林,刘成雁,王志嘉,等.气相色谱-串联质谱法测定土壤中多环芳烃和多氯联苯[J].分析科学学报, 2017,33(2):212-216.
【9】陈晓水,侯宏卫,边照阳,等.气相色谱-串联质谱(GC-MS/MS)的应用研究进展[J].质谱学报, 2013,34(5):308-320.
【10】王丽,金芬,李敏洁,等.分散固相萃取-气相色谱-串联质谱法测定蔬菜中多环芳烃及卤代多环芳烃[J].分析化学, 2013,41(6):869-875.
【11】谢振伟,杨坪,廖翀,等.串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的有机氯农药和多氯联苯[J].中国环境监测, 2008,24(5):20-24.
【12】常君瑞,李娜,徐春雨,等.索氏与超声法提取PM2.5中多环芳烃的比较[J].环境卫生学杂志, 2015,5(2):160-164.
【13】张延平,陈振超,孙晓薇,等.固相萃取/气相色谱-串联质谱法测定竹笋产地土壤中42种持久性有机污染物[J].分析测试学报, 2018,37(12):1431-1438.
【14】马英歌,孙谦,景盛翱,等.超声萃取结合气相色谱三重四极杆质谱联用法测定PM2.5大气污染物中多环芳烃含量[J].环境化学, 2015,34(12):2327-2329.
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