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Determination of lincomycin and tylosin residues in honey by liquid chromatography/tandem mass spectrometry

机译:液相色谱/串联质谱法测定蜂蜜中林可霉素和泰乐菌素的残留量

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A simple and rapid analytical method was developed for the determination of lincomycin and tylosin residues in honey as part of field studies examining the efficacy and target animal safety of these antibiotics to control American foulbrood disease in honey bees. Residues of the antibiotics were determined using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS), Honey samples were diluted and injected directly into the LC/MS/MS system without additional cleanup by solid-phase extraction or liquid-liquid partitioning. A six-port valve system was utilized to selectively route eluant from the LC column into the mass spectrometer only during a relatively short portion of the chromatographic run corresponding to the elution of the analytes of interest. Minimal contamination of the MS source chamber was observed despite the analysis of large numbers of samples. Using internal standard quantitation, excellent accuracy and precision were obtained with no apparent matrix-to-matrix variation. Based on the analysis of fortified replicates, the mean percent deviation from the theoretical concentration and the percent relative standard deviation were both less than 10% for tylosin over an analytical range of 10-1000 mug/kg. Slightly higher mean percent deviations and relative standard deviations were observed for the analysis of lincomycin in fortified replicate samples. The method detection limits were determined to be 5 and 2 mug/kg for lincomycin and tylosin, respectively. Copyright (C)2005 John Wiley Sons, Ltd.
机译:作为现场研究的一部分,开发了一种简单而快速的分析方法,用于测定蜂蜜中的林可霉素和泰乐菌素残留,以检查这些抗生素控制蜜蜂美国的臭脚病的功效和目标动物安全性。使用液相色谱/电喷雾串联质谱法(LC / ESI-MS / MS)确定抗生素的残留量,将蜂蜜样品稀释并直接注入LC / MS / MS系统,而无需通过固相萃取或液体进行额外净化-液体分配。六通阀系统仅在色谱运行相对较短的时间(与目标分析物的洗脱相对应)期间,才将洗脱液从LC色谱柱选择性地引入质谱仪。尽管对大量样品进行了分析,但仍观察到MS源室的污染极小。使用内标定量,可以获得极佳的准确性和精密度,而基质之间没有明显的变化。根据强化重复样品的分析,在10-1000马克杯/千克的分析范围内,泰乐菌素与理论浓度的平均偏差百分数和相对标准偏差百分数均小于10%。在强化重复样品中分析林可霉素时,观察到的平均百分偏差和相对标准偏差略高。对于林可霉素和泰乐菌素,方法检测限分别确定为5和2大杯/千克。版权所有(C)2005 John Wiley Sons,Ltd.

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