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Position: Home > Articles > Detection on the Residues of Lincomycin in Honey by LC-ESI-MS/MS Journal of Anhui Agricultural Sciences 2009,37 (5) 1889-1891

HPLC-ESI-MS/MS检测蜂蜜中林可霉素残留

作  者:
阮祥春;曾明华;赵明
单  位:
安徽农业大学;安徽农业大学动物科技学院
关键词:
蜂蜜;林可霉素;高效液相色谱-电喷雾串联质谱;残留
摘  要:
[目的]建立蜂蜜中林可霉素残留的高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测方法。[方法]样品经固相萃取净化、液相色谱分离后进行质谱分析,在多反应监测模式(MRM)下进行特征母离子、子离子对信号采集。根据保留时间、母离子和两个特征子离子进行定性分析,以离子峰度最强的基峰离子m/z126进行定量。[结果]在1.0~20.0 ng/ml线性范围内,峰强度与添加浓度的线性关系良好(r2>0.9996)。在2.5、5.01、0.0 ng/g 3个添加水平,林可霉素的平均回收率范围为(95.1±3.3)%,日内测定结果的相对标准偏差小于5.3%,日间测定结果的相对标准偏差小于8.5%,最低检测限0.1 ng/g。[结论]HPLC-ESI-MS/MS用作检测蜂蜜中林可霉素残留的方法,灵敏度高、精密度好,达到了林可霉素残留分析的要求。
译  名:
Detection on the Residues of Lincomycin in Honey by LC-ESI-MS/MS
作  者:
RUAN Xiang-chun et al (College of Animal Sciences,Anhui Agricultural University,Hefei,Anhui 230036)
关键词:
Honey;Lincomycin;HPLC-ESI-MS/MS;Residues
摘  要:
[Objective] The purpose was to set up the method of detecting the residues of lincomycin in honey by HPLC-ESI-MS/MS.[Method] The samples purified by solid-phase extraction and isolated by liquid-phase extraction were analyzed by MS.The signal collection of characteristic maternal ions and sub-ion pairs was conducted in MRM.The qualitative analysis was conducted on the basis of retaining time,maternal ions and the two characteristic sub-ions.The quantification was conducted on base-peak ion m/z126,whose ion peak was most intense.[Result] In the linear scope of 1.0-20.0 ng/ml,the peak-intensity had good linear correlation with added concn.(r2>0.999 6).Under the 3 addition levels of 2.5, 5.0 and 10.0 ng/g,the average recovery of lincomycin was(95.1±3.3)%,the RSD of determination results during one day was smaller than 5.3%,that between two days was smaller than 8.5%,with detection limit being 0.1 ng/g.[Conclusion] HPLCESI-MS/MS was a sensitive and precise method in detecting the residues of lincomycin in honey and met the requirements of residues analysis on lincomycin.

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