吹扫捕集-气相色谱-三重四极杆质谱法同时测定水中苯系物和有机含氧汽油添加剂
Simultaneous Determination of BTEX and Gasoline Oxygenates in Water by P&T-GC-QqQ-MS/MS
摘 要
使用吹扫捕集(P&T)和气相色谱-三重四极杆质谱(GC-QqQ-MS/MS)联用仪,建立了同时测定水中12种苯系物和有机含氧汽油添加剂的方法。在US EPA方法8260的基础上对P&T的吹扫温度和解析时间进行了优化,并确定了在多反应监测(MRM)模式下12种待测物的前级离子和产物离子及最优的碰撞能量。12种待测物的线性范围为0.05~20 μg·L-1,检出限(3S/N)在0.52~32 ng·L-1之间,测定下限(10S/N)在1.6~96 ng·L-1之间。加标回收率在80.2%~120%之间。日内(n=5)和日间(n=6)相对标准偏差分别在2.0%~8.9%和1.2~13%之间。
吹扫捕集
苯系物
有机含氧汽油添加剂
水
GC-QqQ-MS/MS
Purge-and-trap
BTEX
Gasoline oxygenates
Water
Abstract
A method for the simultaneous determination of 12 BTEX and gasoline oxygenates in water was developed based on purge-and-trap (P&T) sampling combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS). The parameters of P&T sampling, such as purge temperature and resolution time, were optimized based on the US EPA method 8260. Precursor ions and product ions for the 12 analytes in the multiple reactions monitoring (MRM) mode were identified and the collision energy for the 12 analytes were optimized. The linear ranges of 12 analytes ranged from 0.05 μg·L-1 to 20 μg·L-1 with detection limits (3S/N) in the range of 0.52-32 ng·L-1 and the lower limits of determination (10S/N )in the range of 1.6-96 ng·L-1. Recovery rates obtained by standard addition method were in the ranges of 80.2%-120%, the intra-day RSDs (n=5) and inter-day RSDs (n=6) were in the range of 2.0%-8.9% and 1.2%-13%, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201605030
所属栏目 专题报道(水质分析)
基金项目 国家自然基金项目(51308437);陕西省教育厅基金(2013JK0980);陕西省博士后科学基金
收稿日期 2015/5/7
修改稿日期
网络出版日期
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备注孙 晴(1989-),女,山东济宁人,硕士研究生,主要从事水质监测方法开发研究工作。
引用该论文: SUN Qing,DUAN Jin-ming,LI Wei,LIU Yu-can. Simultaneous Determination of BTEX and Gasoline Oxygenates in Water by P&T-GC-QqQ-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(5): 615～620
孙晴,段晋明,李伟,刘玉灿. 吹扫捕集-气相色谱-三重四极杆质谱法同时测定水中苯系物和有机含氧汽油添加剂[J]. 理化检验－化学分册, 2016, 52(5): 615～620
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参考文献
【1】PAVN J L P, NOGAL S M, LAESPADA M E F, et al. Simultaneous determination of gasoline oxygenates and benzene, toluene, ethylbenzene and xylene in water samples using headspace-programmed temperature vaporization-fast gas chromatography-mass spectrometry［J］. J Chromatogr A, 2007,1175(1): 106-111.
【2】吴金浩,王摆,王召会,等.海水中痕量苯系物的吹扫捕集/气相色谱质谱联用测定［J］.分析测试学报, 2012,31(12): 1531-1535.
【3】ROSELL M, LACORTE S, GINEBREDA A, et al. Simultaneous determination of methyl tert-butyl ether and its degradation products, other gasoline oxygenates and benzene, toluene, ethylbenzene and xylenes in Catalonian groundwater by purge-and-trap-gas chromatography-mass spectrometry［J］. J Chromatogr A, 2003,995(1): 171-184.
【4】ARAMBARRI I, LASA M, GARCIA R, et al. Determination of fuel dialkyl ethers and BTEX in water using headspace solid-phase microextraction and gas chromatography-flame ionization detection［J］. J Chromatogr A, 2004,1033(2): 193-203.
【5】苟德国,黄忠平,陈京京,等.静态顶空气相色谱法测定地表水中苯系物［J］.中国资源综合利用, 2011,29(3): 41-43.
【6】AEPPLI C, BERG M, HOFSTETTER T B, et al. Simultaneous quantification of polar and non-polar volatile organic compounds in water samples by direct aqueous injection-gas chromatography/mass spectrometry［J］. J Chromatogr A, 2008,1181(1/2): 116-124.
【7】陈梅芹,马晓国,吴景雄,等.用于气相色谱分析的样品导入技术及其应用［J］.中国环境监测, 2006,22(1): 32-36.
【8】刘玉灿,段晋明,李伟.气相色谱-三重四级杆质谱联用法同时检测水中10种卤乙酸［J］.分析化学, 2014,42(1): 77-82.
【9】罗永此,英剑波,谢伟宏,等.快速溶剂萃取-气相色谱-串联质谱法测定血中12种催眠类药物［J］.理化检验-化学分册, 2015,51(7): 1014-1017.
【10】BIANCHI F, CARERI M, MARENGO E, et al. Use of experimental design for the purge-and-trap-gaschromatography-mass spectrometry determination of methyl tert-butyl ether, tert-butyl alcohol and BTEX in groundwater at trace level［J］. J Chromatogr A, 2002,975(1): 113-121.
【11】MEZCUA M, AGERA A, HERNANDO M D, et al. Determination of methyl tert-butyl ether and tert-butyl alcohol in seawater samples using purge-and-trap enrichment coupled to gas chromatography with atomic emission and mass spectrometric detection［J］. J Chromatogr A, 2003,999(1/2): 81-90.
【12】LI W, LIU Y C, DUAN J M, et al. Determination of ten haloacetic acids in water using gas chromatography-triple quadrupole mass spectrometry［J］. J Anal Methods, 2013,(5): 2258-2266.
【13】BOLAOS P P, FRENICH A G, VIDAL J L M. Application of gas chromatography-triple quadrupole mass spectrometry in the quantification-confirmation of pesticides and polychlorinated biphenyls in eggs at trace levels［J］. J Chromatogr A, 2007,1167(1): 9-17.
【14】林麒,李俊荣,林坚,等.稳定性同位素内标-吹扫捕集-气相色谱质谱联用分析水中硫化物［J］.分析化学, 2014,42(5): 678-682.
【2】吴金浩,王摆,王召会,等.海水中痕量苯系物的吹扫捕集/气相色谱质谱联用测定［J］.分析测试学报, 2012,31(12): 1531-1535.
【3】ROSELL M, LACORTE S, GINEBREDA A, et al. Simultaneous determination of methyl tert-butyl ether and its degradation products, other gasoline oxygenates and benzene, toluene, ethylbenzene and xylenes in Catalonian groundwater by purge-and-trap-gas chromatography-mass spectrometry［J］. J Chromatogr A, 2003,995(1): 171-184.
【4】ARAMBARRI I, LASA M, GARCIA R, et al. Determination of fuel dialkyl ethers and BTEX in water using headspace solid-phase microextraction and gas chromatography-flame ionization detection［J］. J Chromatogr A, 2004,1033(2): 193-203.
【5】苟德国,黄忠平,陈京京,等.静态顶空气相色谱法测定地表水中苯系物［J］.中国资源综合利用, 2011,29(3): 41-43.
【6】AEPPLI C, BERG M, HOFSTETTER T B, et al. Simultaneous quantification of polar and non-polar volatile organic compounds in water samples by direct aqueous injection-gas chromatography/mass spectrometry［J］. J Chromatogr A, 2008,1181(1/2): 116-124.
【7】陈梅芹,马晓国,吴景雄,等.用于气相色谱分析的样品导入技术及其应用［J］.中国环境监测, 2006,22(1): 32-36.
【8】刘玉灿,段晋明,李伟.气相色谱-三重四级杆质谱联用法同时检测水中10种卤乙酸［J］.分析化学, 2014,42(1): 77-82.
【9】罗永此,英剑波,谢伟宏,等.快速溶剂萃取-气相色谱-串联质谱法测定血中12种催眠类药物［J］.理化检验-化学分册, 2015,51(7): 1014-1017.
【10】BIANCHI F, CARERI M, MARENGO E, et al. Use of experimental design for the purge-and-trap-gaschromatography-mass spectrometry determination of methyl tert-butyl ether, tert-butyl alcohol and BTEX in groundwater at trace level［J］. J Chromatogr A, 2002,975(1): 113-121.
【11】MEZCUA M, AGERA A, HERNANDO M D, et al. Determination of methyl tert-butyl ether and tert-butyl alcohol in seawater samples using purge-and-trap enrichment coupled to gas chromatography with atomic emission and mass spectrometric detection［J］. J Chromatogr A, 2003,999(1/2): 81-90.
【12】LI W, LIU Y C, DUAN J M, et al. Determination of ten haloacetic acids in water using gas chromatography-triple quadrupole mass spectrometry［J］. J Anal Methods, 2013,(5): 2258-2266.
【13】BOLAOS P P, FRENICH A G, VIDAL J L M. Application of gas chromatography-triple quadrupole mass spectrometry in the quantification-confirmation of pesticides and polychlorinated biphenyls in eggs at trace levels［J］. J Chromatogr A, 2007,1167(1): 9-17.
【14】林麒,李俊荣,林坚,等.稳定性同位素内标-吹扫捕集-气相色谱质谱联用分析水中硫化物［J］.分析化学, 2014,42(5): 678-682.
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