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预防医学  2018, Vol. 30 Issue (6): 570-573    DOI: 10.19485/j.cnki.issn2096-5087.2018.06.007
  论著 本期目录 | 过刊浏览 | 高级检索 |
动物性食品中盐酸克仑特罗残留检测色谱条件优化
曹艺耀1,俞顺飞1,宣志强1,赵尧贤1,李新星1,吴寿明1,赵三虎1,刘萍2
1.浙江省疾病预防控制中心,浙江 杭州 310051;
2.山东大学公共卫生学院理化检验学系
Optimization of chromatographic conditions for the determination of clenbuterol hydrochloride residues in animal edible product
CAO Yi-yao,YU Shun-fei,XUAN Zhi-qiang,ZHAO Yao-xian,LI Xin-xing,WU Shou-ming,ZHAO San-hu,LIU Ping
*Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China
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摘要 目的 优化动物性食品中盐酸克仑特罗残留的高效液相色谱法(HPLC)检测条件,建立可大批量测定样品的方法。方法 样品经高氯酸溶液超声提取,乙酸乙酯-异丙醇萃取,有机相浓缩后,采用Agilent C18(150 mm×4.6 mm,5 μm)色谱柱进行分离,流动相为甲醇-磷酸二氢钠溶液,采用高效液相色谱仪进行分析。结果 标准物质在0.2~10.0 μg/mL时,方法的线性关系良好,相关系数(r)=0.999 84;方法的检测限为0.15 μg/kg,低于国标方法的0.5 μg/kg。盐酸克仑特罗保留时间为6.51 min,峰形良好;加标质量为1.6~12 μg时,加标回收率为92.86%~100.93%,高于国标方法(89.79%~92.36%);日内精密度和日间精密度均小于5%,低于国标方法。结论 优化后的色谱条件适用于动物性食品中盐酸克仑特罗的大批量测定。
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曹艺耀
俞顺飞
宣志强
赵尧贤
李新星
吴寿明
赵三虎
刘萍
关键词 高效液相色谱法动物性食品盐酸克仑特罗    
AbstractObjective To establish a high performance liquid chromatography(HPLC)through the optimization of the chromatographic conditions,which can detect the contents of clenbuterol hydrochloride(CL)residues in animal edible product in a large quantity. Methods The animal edible product were extracted by perchloric acid,and then impurities were removed by liquid-liquid extraction(LLE)which used ethyl acetate- isopropanol. After the organic phase was concentrated,C18 column(150 mm×4.6 mm,5 μm)was used to separate CL. Mobile phase were methanol-sodium dihydrogen phosphate,and then determined by HPLC. Results A good linear response was obtained over the range of 0.2-10.0 μg/mL with the correlation coefficient(r)0.999 84. The method determination limit was 0.15 μg/kg which was lower than the National standard method 0.5 μg/kg. The retention time of the CL was 6.51 min,the chromatographic peak was good. The recovery rates spiked with standards 1.6-12 μg were 92.86%-100.93%,which was higher than National standard method(89.79%-92.36%). The precision of intra-day and inter-day were both under 5%,which lower than National standard. Conclusion The optimized chromatographic conditions are suitable for the large quantity determination of clenbuterol hydrochloride in animal edible product.
Key wordsHPLC    Animal edible product    Clenbuterol hydrochloride
          出版日期: 2018-06-04
中图分类号:  R917  
基金资助:浙江省医药卫生科技计划基金项目(2016RCB005)
通信作者: 刘萍,E-mail:liupingp@sdu.edu.cn   
作者简介: 曹艺耀,硕士,医师,主要从事食品安全与风险评估工作
引用本文:   
曹艺耀,俞顺飞,宣志强,赵尧贤,李新星,吴寿明,赵三虎,刘萍. 动物性食品中盐酸克仑特罗残留检测色谱条件优化[J]. 预防医学, 2018, 30(6): 570-573.
CAO Yi-yao,YU Shun-fei,XUAN Zhi-qiang,ZHAO Yao-xian,LI Xin-xing,WU Shou-ming,ZHAO San-hu,LIU Ping. Optimization of chromatographic conditions for the determination of clenbuterol hydrochloride residues in animal edible product. Preventive Medicine, 2018, 30(6): 570-573.
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http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2018.06.007      或      http://www.zjyfyxzz.com/CN/Y2018/V30/I6/570
[1] 曹巧玲,王中民,秦珑,等. 盐酸克伦特罗的毒性、作用机制及其检测方法研究进展[J] . 职业与健康,2011,27(20):2376-2378.
[2] KIM H K,DELLA-FERA M A,HAUSMAN D B,et al. Effect of clenbuterol on apoptosis,adipogenesis,and lipolysis in adipocytes[J] . J Physiol Biochem,2010,66(3):197-203.
[3] ZHANG Q,XIANG J,WANG X,et al. Β2-adrenoceptor agonist clenbuterol reduces infarct size and myocardial apoptosis after myocardial ischaemia/reperfusion in anaesthetized rats[J] . British Journal of Pharmacology,2010,160(6):1561-1572.
[4] 黎源倩. 食品理化检验[M] . 北京:人民卫生出版社,2009: 114-116.
[5] 中华人民共和国卫生部,中国国家标准化管理委员会. 动物性食品中克仑特罗残留量的测定:GB/T 5009.192—2003[S] . 北京:中国标准出版社,2003.
[6] 吴庆洁,石朝晖,蔡江帆. 高效液相色谱法同时测定畜禽组织中4种抗生素及盐酸克伦特罗残留量[J] . 中国卫生检验杂志,2010,20(7):1642-1644.
[7] 何佳璐. 高效液相色谱法测定猪肉中的盐酸克伦特罗[J] . 海峡预防医学杂志,2006,12(2):47-48.
[8] 钱桂平,余建中,王美全,等. 高效液相色谱法检测猪肉盐酸克伦特罗[J] . 现代预防医学,2004,31(4):612-613.
[9] 王春荣,张济,刘岚铮,等. 高效液相色谱法测定猪肉及猪肝中的盐酸克伦特罗[J] . 中国卫生检验杂志,2005,15(1):75-76.
[10] 陈存社,吕会田. 盐酸克伦特罗残留酶联免疫吸附(ELISA)检测方法的研究[J] . 食品与发酵工业,2006,32(7):91-94.
[11] 邹志刚. 盐酸克伦特罗食物中毒及残留检测研究进展[J] . 预防医学论坛,2007,13(2):145-148.
[12] AMENDOLA L,COLAMONICI C,ROSSI F,et al. Determination of clenbuterol in human urine by GC-MS-MS-MS:confirmation analysis in antidoping control[J] . J Chromatogr B Analyt Technol Biomed Life Sci,2002,773(1):7-16.
[13] 滕南雁,刘向红,何颂华,等. 氘代同位素内标液相色谱-串联质谱法测定猪肉、猪肝中8种β受体激动剂类药物残留[J] . 中国卫生检验杂志,2011,21(7):1617-1620.
[14] MELWANKI M B,HUANG S D,FUH M R. Three-phase solvent bar microextraction and determination of trace amounts of clenbuterol in human urine by liquid chromatography and electrospray tandem mass spectrometry[J] . Talanta,2007,72(2):373-377.
[15] 姜艳彬,孙冠如,王海,等. 盐酸克仑特罗胶体金快速检测试纸条的研制[J] . 中国畜牧兽医,2010,37(10):109-113.
[16] 李庆华,陈肖,彭道和,等. 盐酸克伦特罗残留检测方法研究进展[J] . 中国畜牧兽医文摘,2011,27(5):182-183.
[17] 曹艺耀,许崇德,刘萍,等. 动物性食品中喹诺酮类抗生素残留测定[J] . 中国公共卫生,2013,29(10):1450-1452.
[18] 邹学贤. 分析化学[M] . 北京:人民卫生出版社,2008:22-24.
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