在线固相萃取结合高效液相色谱—电喷雾式检测器测定鸡粪中红霉素残留
周茜等
摘 要 将在线固相萃取（online SPE）与高效液相色谱（HPLC）通用型电喷雾检测器（CAD）结合，建立了集约养殖业常用抗生素红霉素的分析方法。5.0 g 鸡粪样品与硅藻土混合后，置于34 mL萃取池中，以热水为萃取剂，在70 ℃、10.4 MPa条件下，用快速溶剂萃取仪提取样品中的红霉素。利用双三元液相色谱仪，采用在线富集进样方式，经Acclaim 120 C18色谱柱，以乙腈0.1%甲酸溶液为流动相分离后，用CAD进行检测。红霉素在21～2000 μg/kg范围内线性关系良好（r≥0.99），检出限为6.3 μg/kg，加标回收率为79.2%～87.5%。
3.4 样品加标回收率
选用不含红霉素的鸡粪为测试对象，在50， 100和150 μg/kg加标浓度下，测定样品的抗生素加标回收率分别为79.2%， 82.6%和87.5%。
3.5 实际样品分析
将从集约养鸡场抽取的10个鸡粪样品按本方法进行处理和检验，结果表明，鸡粪样品中的红霉素谱图见图2。有6个样品有红霉素检出，其中最高含量为1 mg/kg，最低含量为200 μg/kg，说明鸡粪中含有不同程度的红霉素残留。
References
1 Bulletin 235. Ministry of Agriculture of the People′s Republic of China
中华人民共和国农业部公告第235号
2 Official Journal of the European Communities Comminssion Regulation （EC）. No. 1181 / 2002
3 Juhel M， Anger B， Laurentie M. J. AOAC Inter.， 1999， 82（5）： 1046-1053
4 YUE ZhenFeng， CHEN XiaoXia， XIE LiQi， JI CaiNi， HUA HongHui. Chinese J. Anal. Chem.， 2007， 35（9）： 1290-1294
岳振峰， 陈小霞， 谢丽琪， 吉彩霓， 华红慧. 分析化学， 2007， 35（9）： 1290-1294
5 XU JinZhong， WU ZongXian， YANG WenQuan， YANG GongJun， CHEN ZhengXing， DING Tao， SHEN CongYu， WU Bin， JIANG Yuan. Chinese J. Anal. Chem.， 2007， 35（2）： 166-170
徐锦忠， 吴宗贤， 杨雯筌， 杨功俊， 陈正行， 丁 涛， 沈崇钰， 吴 斌， 蒋 原. 分析化学， 2007， 35（2）： 166-170
6 Draisic R， Palleschi L， Ferretti E， Achene L， Cecilia A. J. Chromatogr. A， 2001， 926（1）： 97-104
7 LI Yan， SHAO Bing， XU SuoHong. Chinese Journal of Heathy Laboratory， 2005， 15（10）： 1275-1277
李 岩， 邵 兵， 徐锁洪. 中国卫生检验杂志， 2005， 15（10）： 1275-1277
8 YU HuiJuan， SHEN XiaoSheng， LI Qing， HUANG DongMei， CHEN YiNan， GUAN LeDong. Chinese Journal of Analysis Laboratory， 2006， 25（4）： 82-85
于慧娟， 沈晓盛， 李 庆， 黄冬梅， 陈轶男， 菅乐东. 分析试验室， 2006， 25（4）： 82-85
9 JIANG QingWei， YANG Rui， MEI XingGuo. Chinese Pharmaceutical Journal， 2007， 42（23）： 1794-1796
姜庆伟， 杨 瑞， 梅兴国. 中国药学杂志， 2007， 42（23）： 1794-1796
10 Moreau R A. Lipid Tech.， 2009， 21（89）： 191-194
11 Zhang K， Dai L， Chetwyn N P. J. Chromatogr. A， 2010， 1217（37）： 5776-5784
12 Blasco C， Corcla AD， Picó Y. Food Chem.， 2009， 116（4）： 1005-1012
Determination of Erythrocin in Chicken Manure by High Performance
Liquid ChromatographyCoronaCharged Aerosol Detection
Coupled with Online Solid Phase Extraction
ZHOU Qian1， CHEN ManTang1， ZHU LiHua1， DING Yao Bin2
1（College of Chemistry and Chemical Engineering， Huazhong University of Science and Technology， Wuhan 430074， China）
2（College of Chemistry and Material Science， SouthCentral University for Nationalities， Wuhan 430074， China）
Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.
Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction
（Received 25 August 2014； accepted 8 October 2014）
This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）
Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.
Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction
（Received 25 August 2014； accepted 8 October 2014）
This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）
Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.
Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction
（Received 25 August 2014； accepted 8 October 2014）
This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）
摘 要 将在线固相萃取（online SPE）与高效液相色谱（HPLC）通用型电喷雾检测器（CAD）结合，建立了集约养殖业常用抗生素红霉素的分析方法。5.0 g 鸡粪样品与硅藻土混合后，置于34 mL萃取池中，以热水为萃取剂，在70 ℃、10.4 MPa条件下，用快速溶剂萃取仪提取样品中的红霉素。利用双三元液相色谱仪，采用在线富集进样方式，经Acclaim 120 C18色谱柱，以乙腈0.1%甲酸溶液为流动相分离后，用CAD进行检测。红霉素在21～2000 μg/kg范围内线性关系良好（r≥0.99），检出限为6.3 μg/kg，加标回收率为79.2%～87.5%。
3.4 样品加标回收率
选用不含红霉素的鸡粪为测试对象，在50， 100和150 μg/kg加标浓度下，测定样品的抗生素加标回收率分别为79.2%， 82.6%和87.5%。
3.5 实际样品分析
将从集约养鸡场抽取的10个鸡粪样品按本方法进行处理和检验，结果表明，鸡粪样品中的红霉素谱图见图2。有6个样品有红霉素检出，其中最高含量为1 mg/kg，最低含量为200 μg/kg，说明鸡粪中含有不同程度的红霉素残留。
References
1 Bulletin 235. Ministry of Agriculture of the People′s Republic of China
中华人民共和国农业部公告第235号
2 Official Journal of the European Communities Comminssion Regulation （EC）. No. 1181 / 2002
3 Juhel M， Anger B， Laurentie M. J. AOAC Inter.， 1999， 82（5）： 1046-1053
4 YUE ZhenFeng， CHEN XiaoXia， XIE LiQi， JI CaiNi， HUA HongHui. Chinese J. Anal. Chem.， 2007， 35（9）： 1290-1294
岳振峰， 陈小霞， 谢丽琪， 吉彩霓， 华红慧. 分析化学， 2007， 35（9）： 1290-1294
5 XU JinZhong， WU ZongXian， YANG WenQuan， YANG GongJun， CHEN ZhengXing， DING Tao， SHEN CongYu， WU Bin， JIANG Yuan. Chinese J. Anal. Chem.， 2007， 35（2）： 166-170
徐锦忠， 吴宗贤， 杨雯筌， 杨功俊， 陈正行， 丁 涛， 沈崇钰， 吴 斌， 蒋 原. 分析化学， 2007， 35（2）： 166-170
6 Draisic R， Palleschi L， Ferretti E， Achene L， Cecilia A. J. Chromatogr. A， 2001， 926（1）： 97-104
7 LI Yan， SHAO Bing， XU SuoHong. Chinese Journal of Heathy Laboratory， 2005， 15（10）： 1275-1277
李 岩， 邵 兵， 徐锁洪. 中国卫生检验杂志， 2005， 15（10）： 1275-1277
8 YU HuiJuan， SHEN XiaoSheng， LI Qing， HUANG DongMei， CHEN YiNan， GUAN LeDong. Chinese Journal of Analysis Laboratory， 2006， 25（4）： 82-85
于慧娟， 沈晓盛， 李 庆， 黄冬梅， 陈轶男， 菅乐东. 分析试验室， 2006， 25（4）： 82-85
9 JIANG QingWei， YANG Rui， MEI XingGuo. Chinese Pharmaceutical Journal， 2007， 42（23）： 1794-1796
姜庆伟， 杨 瑞， 梅兴国. 中国药学杂志， 2007， 42（23）： 1794-1796
10 Moreau R A. Lipid Tech.， 2009， 21（89）： 191-194
11 Zhang K， Dai L， Chetwyn N P. J. Chromatogr. A， 2010， 1217（37）： 5776-5784
12 Blasco C， Corcla AD， Picó Y. Food Chem.， 2009， 116（4）： 1005-1012
Determination of Erythrocin in Chicken Manure by High Performance
Liquid ChromatographyCoronaCharged Aerosol Detection
Coupled with Online Solid Phase Extraction
ZHOU Qian1， CHEN ManTang1， ZHU LiHua1， DING Yao Bin2
1（College of Chemistry and Chemical Engineering， Huazhong University of Science and Technology， Wuhan 430074， China）
2（College of Chemistry and Material Science， SouthCentral University for Nationalities， Wuhan 430074， China）
Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.
Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction
（Received 25 August 2014； accepted 8 October 2014）
This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）
Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.
Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction
（Received 25 August 2014； accepted 8 October 2014）
This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）
Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.
Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction
（Received 25 August 2014； accepted 8 October 2014）
This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）
