HPLC Determination of Residual Amounts of Clenbuterol in Pork and Serum
摘 要
采用高效液相色谱法测定了猪肉及血清中盐酸克伦特罗残留量。样品经甲醇-盐酸混合液提取,乙二胺-N-丙基硅烷净化后,采用Zorbax Eclipse C18色谱柱分离,以甲醇-0.01 mol·L-1磷酸二氢钠(68+32)混合液为流动相进行洗脱,在波长270 nm处进行紫外检测。盐酸克伦特罗的线性范围为0.01~5.00 mg·L-1,检出限(3S/N)为1.8 μg·kg-1,加标回收率在87.4%~99.2%之间,测定值的相对标准偏差(n=5)在2.1%~2.8%之间。
Abstract
HPLC was applied to the determination of residual amounts of clenbuterol in pork and serum. The sample was extracted with a mixture of methanol and 0.01 mol·L-1 hydrochloric acid (68+32) and after purification with ethylenediamine-N-propylsilane, the sample solution was separated on Zorbax Eclipse C18 chromatographic column with a mixture of methanol and sodium dihydrogen phosphate solution (68+32) as mobile phase. UV detection was made at the wavelength of 270 nm. Linearity range of clenbuterol was between 0.01-5.00 mg·L-1, with detection limit (3S/N) of 1.8 μg·kg-1. Values of recovery obtained by standard addition method were in the range of 87.4%-99.2% , with RSDs (n=5) in the range of 2.1%-2.8%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201512012
所属栏目 工作简报
基金项目 山东省自然基金项目(ZR2011BM009)
收稿日期 2014/12/11
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备注李娜(1990-),女,江苏徐州人,硕士研究生,研究 方向样品前处理、食品及农药残留分析。
引用该论文: LI Na,LIU Pei-pei,LI Gui-zhi,LIU Yong-ming. HPLC Determination of Residual Amounts of Clenbuterol in Pork and Serum[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(12): 1684~1688
李娜,刘佩佩,李桂芝,刘永明. 高效液相色谱法测定猪肉及血清中盐酸克伦特罗残留量[J]. 理化检验-化学分册, 2015, 51(12): 1684~1688
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参考文献
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【2】SONG Jing-jing, XU Ming-xia, ZHAO Kang, et al. Flow injection chemiluminescence immunosensor for the determination of clenbuterol by immobilizing coating-antigen on carboxylic resin beads[J]. Analytical Methods, 2014,6(9):3152-3158.
【3】LI Li-jun, ZHANG Jun-min, TANG Chao-hua, et al. Accumulation of clenbuterol residues in the hair of Chinese simmental beef cattle during and after treatment[J]. Journal of Analytical Toxicology, 2014,38(1):52-56.
【4】MANISH Y, VIKAS T, VIVEK U, et al. Comparison of extraction procedures for assessment of matrix effect for selective and reliable determination of atazanavir in human plasma by LC-ESI-MS/MS[J]. Journal of Chromatography B, 2012,885:138-149.
【5】LIU Bao-mi, YAN Hong-yuan, QIAO Feng-xia, et al. Determination of clenbuterol in porcine tissues using solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and HPLC-UV detection[J]. Journal of Chromatography B, 2011,879(1):90-94.
【6】DENG Qiao-qiao, LI Gui-zhi, LIU Pei-pei, et al. Effects of protein on the detection of chlorobenzenes in fish and their elimination by modified QuEChERS method[J]. Chemical Research in Chinese Universities, 2013,29(6):1063-1067.
【7】JIA Feng-yan, WANG Wen-wen, WANG Juan, et al. New strategy to enhance the extraction efficiency of pyrethroid pesticides in fish samples using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method[J]. Analytical Methods, 2012,4(2):449-453.
【8】ZHANG Xing-mei, DENG Qiao-qiao, LIU Pei-pei, et al. Effect of protein on the detection of stilbene estrogens in milk[J]. Analytical Methods, 2014(6):2276-2281.
【9】潘祖亭,马勇,王巍.荧光光谱法研究克伦特罗与蛋白质的结合作用[J].分析试验室, 2004,23(1):5-8.
【10】WANG Wen-wen, GAO Fu-kai, LI Gui-zhi, et al. High efficient extraction of phthalates in aquatic products by a modified QuEChERS method[J]. Chemical Research in Chinese Univercities, 2013,29(4):653-656.
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