分子印迹固相萃取-超高效液相色谱串联质谱法测定猪肉中磺胺二甲氧嗪
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摘要
建立了基于分子印迹聚合物(MIPs)为固相萃取填料的固相萃取技术结合超高效液相色谱串联质谱法(MISPE-UPLC-MS/MS)检测猪肉中磺胺二甲氧嗪。以磺胺二甲氧嗪为模板分子,三氟甲基丙烯酸为功能单体,采用沉淀聚合法制备了分子印迹固相萃取填料,并对萃取净化条件进行了优化。在优化的提取条件和分析条件下,对猪肉肌肉样品中磺胺二甲氧嗪进行分析,其检出限为1.225μg/kg;定量限为4.083μg/kg;双水平回收率在81.4%~106.9%;RSD为3.7%和12%。与M CX柱净化相比,分子印迹固相萃取柱能够有效去除基质效应,分离待测物与杂质。
A method was developed for the detection of sulfadimethoxine( SDM') in pork by ultra performance liquid chromatography tandem mass spectrometry with molecularly imprinted solid phase extraction( MISPE-UPLC-MS/MS) based on molecularly imprinted polymer( MIPs) which were prepared via precipitation polymerization with 2-( trifluoromethyl) acrylic acid as functional monomers.The conditions of solid phase extraction and purification were optimized. A better enrichment and purification effect as well as removing matrix effect significantly was showed by solid phase extraction with MIPs than MCX for pork muscle samples. On the basis of the optimization of sample extraction and separation enrichment methods, the method detection limit and quantification limit were1. 225 μg/kg and 4. 083 μg/kg respectively. The bi-level recoveries were 81. 4% ~ 106. 9%; RSDs were 3. 7% and 12%,respectively. Compared with the MCX purification,the molecularly imprinted solid phase extraction can remove the matrix effect, and separate the analytes from impurities effectively.
A method was developed for the detection of sulfadimethoxine( SDM') in pork by ultra performance liquid chromatography tandem mass spectrometry with molecularly imprinted solid phase extraction( MISPE-UPLC-MS/MS) based on molecularly imprinted polymer( MIPs) which were prepared via precipitation polymerization with 2-( trifluoromethyl) acrylic acid as functional monomers.The conditions of solid phase extraction and purification were optimized. A better enrichment and purification effect as well as removing matrix effect significantly was showed by solid phase extraction with MIPs than MCX for pork muscle samples. On the basis of the optimization of sample extraction and separation enrichment methods, the method detection limit and quantification limit were1. 225 μg/kg and 4. 083 μg/kg respectively. The bi-level recoveries were 81. 4% ~ 106. 9%; RSDs were 3. 7% and 12%,respectively. Compared with the MCX purification,the molecularly imprinted solid phase extraction can remove the matrix effect, and separate the analytes from impurities effectively.
引文
[1]ZHONG Lingli,LEI Shaorong,GUO Lingan,et al.Chin J Anal Lab,2016,35(1):51仲伶俐,雷绍荣,郭灵安,等.分析试验室,2016,35(1):51
[2]LUO Huitai,HUANG Xiaolan,WU Huiqin,et al.J Instrum Anal,2015,34(9):979罗辉泰,黄晓兰,吴惠勤,等.分析测试学报,2015,34(9):979
[3]YANG Dongdong,CONG Lujing,TIAN Mingming,et al.Chin J Anal Chem,2015,34(9):872杨东冬,丛路静,田明明,等.分析化学,2015,34(9):872
[4]Xie R F,Hu Q F,Yang G Y,et al.Rare Met,2016,35(3):282
[5]QIN Shili,SU Liqiang,WANG Peng.Chin J Anal Lab,2016,35(5):590秦世丽,苏立强,王鹏.分析试验室,2016,35(5):590
[6]Majid Soleimani,Majid Ghahraman Afshar.J Anal Chem,2015,70(1):5
[7]WANG Lijun,CAO Xumin,SUN Xiaoliang,et al.Chin J Chromatogr,2016,34(3):240王丽君,曹旭敏,孙晓亮,等.色谱,2016,34(3):240
[8]Polyanina D A,Beklemishev M K.J Anal Chem,2015,70(3):277
[9]LI Rong,CHU Dake,GAO Yongqing,et al.Chin J Anal Lab,2015,34(8):907李蓉,储大可,高永清,等.分析试验室,2015,34(8):907
[10]TANG Kaijie,LUO Qiushui,YU Ruilong,et al.J Instrum Anal,2016,35(1):115汤凯杰,罗秋水,余瑞龙,等.分析测试学报,2016,35(1):115
[11]ZUO Haigen,XING Ming,GUO Ping,et al.Chin J Anal Lab,2015,34(10):1187左海根,幸明,郭平,等.分析试验室,2015,34(10):1187
[12]Shang Y Z,Luo J,Wang P,et al.J Anal Meth Chem,2016,2016(1):1
[13]MEI Xiaoxin,HE Xiuping,WANG Jiangtao.Chin J Anal Chem,2016,44(2):212梅晓欣,何秀平,王江涛.分析化学,2016,44(2):212
[14]LI Jin-cheng,ZHANG Jing,LIU Yang.Anal Bioanal Chem,2015,407(21):6563
[2]LUO Huitai,HUANG Xiaolan,WU Huiqin,et al.J Instrum Anal,2015,34(9):979罗辉泰,黄晓兰,吴惠勤,等.分析测试学报,2015,34(9):979
[3]YANG Dongdong,CONG Lujing,TIAN Mingming,et al.Chin J Anal Chem,2015,34(9):872杨东冬,丛路静,田明明,等.分析化学,2015,34(9):872
[4]Xie R F,Hu Q F,Yang G Y,et al.Rare Met,2016,35(3):282
[5]QIN Shili,SU Liqiang,WANG Peng.Chin J Anal Lab,2016,35(5):590秦世丽,苏立强,王鹏.分析试验室,2016,35(5):590
[6]Majid Soleimani,Majid Ghahraman Afshar.J Anal Chem,2015,70(1):5
[7]WANG Lijun,CAO Xumin,SUN Xiaoliang,et al.Chin J Chromatogr,2016,34(3):240王丽君,曹旭敏,孙晓亮,等.色谱,2016,34(3):240
[8]Polyanina D A,Beklemishev M K.J Anal Chem,2015,70(3):277
[9]LI Rong,CHU Dake,GAO Yongqing,et al.Chin J Anal Lab,2015,34(8):907李蓉,储大可,高永清,等.分析试验室,2015,34(8):907
[10]TANG Kaijie,LUO Qiushui,YU Ruilong,et al.J Instrum Anal,2016,35(1):115汤凯杰,罗秋水,余瑞龙,等.分析测试学报,2016,35(1):115
[11]ZUO Haigen,XING Ming,GUO Ping,et al.Chin J Anal Lab,2015,34(10):1187左海根,幸明,郭平,等.分析试验室,2015,34(10):1187
[12]Shang Y Z,Luo J,Wang P,et al.J Anal Meth Chem,2016,2016(1):1
[13]MEI Xiaoxin,HE Xiuping,WANG Jiangtao.Chin J Anal Chem,2016,44(2):212梅晓欣,何秀平,王江涛.分析化学,2016,44(2):212
[14]LI Jin-cheng,ZHANG Jing,LIU Yang.Anal Bioanal Chem,2015,407(21):6563