摘要
目的建立蜂蜜中林可霉素残留的高效液相色谱-质谱联用法,并用于江苏五市市售蜂蜜中林可霉素的残留水平检测。方法样品经固相萃取提取净化、反相液相色谱分离后质谱检测,基质匹配标准内标法定量。结果方法在1.0μg/kg~100μg/kg浓度时线性关系良好(r=0.996),检出限为0.2μg/kg,定量限为0.7μg/kg,回收率为92.88%~107.51%,相对标准偏差为4.6%~8.6%。样品中林可霉素的检出率为24%,最大残留量为2.998μg/kg。结论该法简单、灵敏、准确,可用于蜂蜜中林可霉素残留的测定。
Objective To develop an analytical method for the determination of lincomycin in honey by ultra performance liquid chromatography-tandem mass spectrometry and apply the method to the investigation of lincomycin residue in honey from five cities of Jiangsu Province. Methods The sample was extracted and purified with solid-phase extraction and then separated with reversed-phase ultra performance liquid chromatography and detected by electro spray tandem mass spectrometry in the MRM mode. Quantification was based on internal standard with matrix-matched calibration standard curve. Results The linearity for lincomycin ranged from 1.0 μg/kg-100 μg/kg with the correlation coefficient(r) greater than 0.996. The limit of detection(LOD) of lincomycin was 0.2 μg/kg, and the limit of quantification(LOQ) was 0.7 μg/kg. The recoveries were within 92.88%-107.51% with the relative standard deviations of 4.6%-8.6%. The positive rate of lincomycin in 50 samples was 24%, and the highest content was 2.998 μg/kg. Conclusion The method is simple, sensitive, accurate, and it can be applied to the determination of lincomycin in honey.
引文
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