在线净化液相色谱串联质谱法测定畜禽粪便中

李丹妮等
摘 要 建立了同时测定畜禽粪便中福莫特罗、沙美特罗、卡布特罗、克伦异磅特罗、克伦潘特、克伦塞罗和羟甲基克伦特罗7种β2受体激动剂的超高效液相色谱发现, 随着提取液中有机相比例提高,化合物的提取效率也相应提高,选择酸性乙腈作为提取剂时,7种β2受体激动剂提取效果均比较理想。
3.3 在线固相萃取条件的优化
畜禽粪便是一种成分复杂的生物样品基质。畜禽养殖场粪便成分中水分占3/4,其余为固体成分,为死细菌、脂肪、蛋白质、无机盐及未消化固体成分[ 21]。此外还含有大量会对兽药产生较强的吸附力的有机质[ 22],这些均会带来较大的基质效应,干扰猪粪便样品中目标物检测。目前文献报道畜禽粪便中的前处理方式多为离线固相萃取,操作相对复杂,时间长,本研究采用双三元液相系统,开发了一种在线SPE净化方法,大大节省了前处理时间,简化了前处理步骤。
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孟盼盼. 科技信息, 2009, (20): 429
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孙 刚, 袁守军, 计 峰, 彭书传, 胡真虎. 环境与健康杂志, 2009, 26(3): 277
Simultaneous Determination of Seven β2Agonists in
Livestock Manure by Online Cleanup Liquid
ChromatographyTandem Mass Spectrometry
LI DanNi*, YAN Feng, WU JianPing, ZHOU YueRong, GU Xin, ZHANG Xin
(Shanghai Animal Disease Control Center, Shanghai 201103, China)
Abstract A new method using online cleanup technology combined with liquid chromatography tandem mass spectrometry (UHPLCMS/MS) was developed for the determination of seven kinds of β2agonists residues, Formoterol, Salmeterol, Carbuterol, Clenisopenterol, Clenpenterol, Clencyclohexerol and Clenbuterolhydroxymethyl in livestock manure. The sample was sufficiently extracted by acidic acetonitrile and diluted by 0.2% formic acid. The extract was online purified on HyperSep Retain CX column where the sample matrix was washed away and the analytes were retained.The analytes were eluted into Hypersil Gold C18 column by 2% Ammoniamethanol solution. The seven β2agonists were detected in selected reaction monitoring (SRM) mode via positive electrospray ionization (ESI+) by liquid chromatographytandem mass spectrometry. The results showed good linearity correlation coefficients over 0.9928 for the seven kinds of β2agonists in 0.5-100 μg/L concentration range. The LOD of seven kinds of β2agonists in livestock mature is 1 μg/kg, while the LOQ is 5 μg/kg. When 5-50 μg/kg of the seven kinds of β2agonists were added into the blank livestock manure, an average recovery of 67% -112% was obtained with the relative standard deviations of 2.9%-10.2%. The method is simple, rapid and has good reproducibility for quantitative and confirmatory analysis of β2agonist residues.
Keywords Online cleanup liquid chromatographytandem mass spectrometry; Seven β2 agonists; Residue; Livestock manure
(Received 20 August 2014; accepted 8 October 2014)
13 WANG PeiLong, FAN Li, SU XiaoOu, YE ZhiHua. Chinese J. Anal. Chem., 2012, 40(3): 470-473
王培龙, 范理, 苏晓鸥, 叶志华. 分析化学, 2012, 40(3): 470-473
14 LIN YiZhi, LIU Fen, DAI JingJing, LIANG Wei. Chinese Journal of Health Laboratory Technology, 2002, 12(2): 180-181
林奕芝, 刘 奋, 戴京晶, 梁 伟. 中国卫生检验杂志, 2002, 12(2): 180-181
15 Suhui S, Jin O, Willy R.G. B, Joris R. Delanghec, Yiping Y. J. Pharmaceu. Biomed. Anal., 2005, 38: 166-172
16 HingBiu Lee, Kurtis S, Thomas E. P. J. Chromatogr. A, 2007, 1148: 158-167
17 LI Yang, SU XiaoOu, WANG RuiGuo, WANG PeiLong, ZHANG Wei, CHEN Jie. Chinese J. Anal. Chem., 2013, 41(6): 899-904
李 阳, 苏晓鸥, 王瑞国, 王培龙, 张 维, 程 劼. 分析化学, 2013, 41(6): 899-904
18 XIANGDang Dua, YINLiang Wub, HONGJu Yangc, TING Y. J. Chromatogr. A, 2012, 1260: 25-32
19 DUAN YongSheng, WANG BingLing, AI LianFeng, GUO ChunHai, GE ShiHui, ZHANG JingWen, XU NiuSheng. Chinese J.Chromatogr., 2014, 32(6): 647-652
段永生, 王炳玲, 艾连峰, 郭春海, 葛世辉, 张婧雯, 徐牛生. 色谱, 2014, 32(6): 647-652
20 AI LianFeng, MA YuSong, CHEN RuiChun,GUO ChunHai, KANG ZhanSheng. Chinese J. Anal. Chem., 2013, 41(8): 1194-1198
艾连峰, 马育松, 陈瑞春, 郭春海, 康占省. 分析化学, 2013, 41(8): 1194-1198
21 MENG PanPan. Science & Technology Information., 2009, (20): 429
孟盼盼. 科技信息, 2009, (20): 429
22 SUN Gang, YUAN ShouJun, JI Feng, PENG ShuChuan, HU ZhenHu. Journal of Environment and Health, 2009, 26(3): 277
孙 刚, 袁守军, 计 峰, 彭书传, 胡真虎. 环境与健康杂志, 2009, 26(3): 277
Simultaneous Determination of Seven β2Agonists in
Livestock Manure by Online Cleanup Liquid
ChromatographyTandem Mass Spectrometry
LI DanNi*, YAN Feng, WU JianPing, ZHOU YueRong, GU Xin, ZHANG Xin
(Shanghai Animal Disease Control Center, Shanghai 201103, China)
Abstract A new method using online cleanup technology combined with liquid chromatography tandem mass spectrometry (UHPLCMS/MS) was developed for the determination of seven kinds of β2agonists residues, Formoterol, Salmeterol, Carbuterol, Clenisopenterol, Clenpenterol, Clencyclohexerol and Clenbuterolhydroxymethyl in livestock manure. The sample was sufficiently extracted by acidic acetonitrile and diluted by 0.2% formic acid. The extract was online purified on HyperSep Retain CX column where the sample matrix was washed away and the analytes were retained.The analytes were eluted into Hypersil Gold C18 column by 2% Ammoniamethanol solution. The seven β2agonists were detected in selected reaction monitoring (SRM) mode via positive electrospray ionization (ESI+) by liquid chromatographytandem mass spectrometry. The results showed good linearity correlation coefficients over 0.9928 for the seven kinds of β2agonists in 0.5-100 μg/L concentration range. The LOD of seven kinds of β2agonists in livestock mature is 1 μg/kg, while the LOQ is 5 μg/kg. When 5-50 μg/kg of the seven kinds of β2agonists were added into the blank livestock manure, an average recovery of 67% -112% was obtained with the relative standard deviations of 2.9%-10.2%. The method is simple, rapid and has good reproducibility for quantitative and confirmatory analysis of β2agonist residues.
Keywords Online cleanup liquid chromatographytandem mass spectrometry; Seven β2 agonists; Residue; Livestock manure
(Received 20 August 2014; accepted 8 October 2014)
13 WANG PeiLong, FAN Li, SU XiaoOu, YE ZhiHua. Chinese J. Anal. Chem., 2012, 40(3): 470-473
王培龙, 范理, 苏晓鸥, 叶志华. 分析化学, 2012, 40(3): 470-473
14 LIN YiZhi, LIU Fen, DAI JingJing, LIANG Wei. Chinese Journal of Health Laboratory Technology, 2002, 12(2): 180-181
林奕芝, 刘 奋, 戴京晶, 梁 伟. 中国卫生检验杂志, 2002, 12(2): 180-181
15 Suhui S, Jin O, Willy R.G. B, Joris R. Delanghec, Yiping Y. J. Pharmaceu. Biomed. Anal., 2005, 38: 166-172
16 HingBiu Lee, Kurtis S, Thomas E. P. J. Chromatogr. A, 2007, 1148: 158-167
17 LI Yang, SU XiaoOu, WANG RuiGuo, WANG PeiLong, ZHANG Wei, CHEN Jie. Chinese J. Anal. Chem., 2013, 41(6): 899-904
李 阳, 苏晓鸥, 王瑞国, 王培龙, 张 维, 程 劼. 分析化学, 2013, 41(6): 899-904
18 XIANGDang Dua, YINLiang Wub, HONGJu Yangc, TING Y. J. Chromatogr. A, 2012, 1260: 25-32
19 DUAN YongSheng, WANG BingLing, AI LianFeng, GUO ChunHai, GE ShiHui, ZHANG JingWen, XU NiuSheng. Chinese J.Chromatogr., 2014, 32(6): 647-652
段永生, 王炳玲, 艾连峰, 郭春海, 葛世辉, 张婧雯, 徐牛生. 色谱, 2014, 32(6): 647-652
20 AI LianFeng, MA YuSong, CHEN RuiChun,GUO ChunHai, KANG ZhanSheng. Chinese J. Anal. Chem., 2013, 41(8): 1194-1198
艾连峰, 马育松, 陈瑞春, 郭春海, 康占省. 分析化学, 2013, 41(8): 1194-1198
21 MENG PanPan. Science & Technology Information., 2009, (20): 429
孟盼盼. 科技信息, 2009, (20): 429
22 SUN Gang, YUAN ShouJun, JI Feng, PENG ShuChuan, HU ZhenHu. Journal of Environment and Health, 2009, 26(3): 277
孙 刚, 袁守军, 计 峰, 彭书传, 胡真虎. 环境与健康杂志, 2009, 26(3): 277
Simultaneous Determination of Seven β2Agonists in
Livestock Manure by Online Cleanup Liquid
ChromatographyTandem Mass Spectrometry
LI DanNi*, YAN Feng, WU JianPing, ZHOU YueRong, GU Xin, ZHANG Xin
(Shanghai Animal Disease Control Center, Shanghai 201103, China)
Abstract A new method using online cleanup technology combined with liquid chromatography tandem mass spectrometry (UHPLCMS/MS) was developed for the determination of seven kinds of β2agonists residues, Formoterol, Salmeterol, Carbuterol, Clenisopenterol, Clenpenterol, Clencyclohexerol and Clenbuterolhydroxymethyl in livestock manure. The sample was sufficiently extracted by acidic acetonitrile and diluted by 0.2% formic acid. The extract was online purified on HyperSep Retain CX column where the sample matrix was washed away and the analytes were retained.The analytes were eluted into Hypersil Gold C18 column by 2% Ammoniamethanol solution. The seven β2agonists were detected in selected reaction monitoring (SRM) mode via positive electrospray ionization (ESI+) by liquid chromatographytandem mass spectrometry. The results showed good linearity correlation coefficients over 0.9928 for the seven kinds of β2agonists in 0.5-100 μg/L concentration range. The LOD of seven kinds of β2agonists in livestock mature is 1 μg/kg, while the LOQ is 5 μg/kg. When 5-50 μg/kg of the seven kinds of β2agonists were added into the blank livestock manure, an average recovery of 67% -112% was obtained with the relative standard deviations of 2.9%-10.2%. The method is simple, rapid and has good reproducibility for quantitative and confirmatory analysis of β2agonist residues.
Keywords Online cleanup liquid chromatographytandem mass spectrometry; Seven β2 agonists; Residue; Livestock manure
(Received 20 August 2014; accepted 8 October 2014)
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