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高效液相色谱法测定脂肪中11种苯并咪唑类药物残留标志物
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作者单位
邵琳智,邹游,陈思敏 广东检验检疫技术中心 
基金项目:农业行业修制定标准项目(2017-108)
中文摘要:建立了同时测定脂肪中11种苯并咪唑类药物残留标志物的高效液相色谱法。样品采用正己烷溶解后,加入抗氧化剂,用0.1 mol/L盐酸-乙腈(1∶1,体积比)提取,经正己烷脱脂后再次加入抗氧化剂,以MCX固相萃取柱净化。净化液浓缩处理后进行高效液相色谱分离,以甲醇-1%乙酸为流动相梯度洗脱,流速为1.0 mL/min,紫外检测波长为292 nm,采用外标法以峰面积定量检测。11种目标物均在25.0~1 000 μg/L范围内线性良好,方法定量下限为50 μg/kg,在3个加标水平下的回收率为82.0%~109%,相对标准偏差(RSD)为0.71%~9.9%。该方法能够满足脂肪中苯并咪唑类药物残留标志物的检测要求。
中文关键词:苯并咪唑类药物残留标志物  脂肪  固相萃取  高效液相色谱法
 
Determination of 11 Benzimidazoles Metabolites Residues in Fat by High Performance Liquid Chromatography
Abstract:A high performance liquid chromatographic method was developed for the simultaneous determination of 11 benzimidazoles metabolites residues in fat.Samples were firstly dissolved with n hexane,then extracted with antioxidant and 0.1 mol/L hydrochloric acid-acetonitrile(1∶1,by volume),followed by treatments with n hexane for defatting,antioxidant again and further clean-up on a MCX solid phase extraction(SPE) column.After concentration,the chromatographic separation was performed on an Atlantis T3 column by gradient elution with a mixed solution of methanol and 1%acetic acid at a flow rate of 1.0 mL/min.The detection wavelength was set at 292 nm,and the external standard method was used for quantitation.The calibration curves for 11 analytes were linear in the range of 25.0-1 000 μg/L with quantitation limits of 50 μg/kg.The recoveries at three spiked levels ranged from 82.0%to 109%with relative standard deviations(RSD) of 0.71%-9.9%.The developed method could meet the requirements for determination of 11 benzimidazoles metabolites residues in fat.
Key Words:benzimidazoles metabolites residues  fat  solid phase extraction  high performance liquid chromatography
引用本文:邵琳智,邹游,陈思敏.高效液相色谱法测定脂肪中11种苯并咪唑类药物残留标志物[J].分析测试学报,2019,(8):990-994.
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