| 氧化锌QuEChERS/高效液相色谱-串联质谱法测定蜂蜜中7种林可酰胺类与大环内酯类兽药残留 |
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| 基金项目:湖北省自然科学基金计划项目(2018CFB340) |
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| 中文摘要:建立了高效液相色谱-串联质谱(HPLC-MS/MS)快速测定蜂蜜中7种林可酰胺类和大环内酯类兽药残留的方法。样品采用磷酸盐缓冲液(pH 8.0)溶解，1%氨水乙腈提取，无水硫酸钠盐析，以80 mg ZnO+20 mg PSA净化。以0.1%甲酸水和乙腈为流动相，采用Waters XBridge C18(150 mm×2.1 mm，5 μm)色谱柱进行分离，电喷雾电离正离子模式(ESI+)扫描，多反应监测(MRM)模式检测，基质匹配标准溶液外标法定量。结果表明，7种目标化合物在各自的质量浓度范围内呈良好线性，相关系数(r)均不小于0.999 3，方法检出限为0.21~0.35 μg/kg，定量下限为0.69~1.16 μg/kg；在3个加标水平(5.0、10.0、20.0 μg/kg)下的平均回收率为75.5%~99.0%，相对标准偏差为0.78%~5.9%。该方法简便快速、灵敏度高、重现性好，能满足蜂蜜中7种林可酰胺类和大环内酯类兽药残留的快速检测要求。 |
| 中文关键词:蜂蜜 高效液相色谱-串联质谱(HPLC-MS/MS) 林可酰胺类兽药 大环内酯类兽药 氧化锌 QuEChERS |
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| Determination of Seven Lincosamides and Macrolides Residues in Honeys by High Performance Liquid Chromatography-Tandem Mass Spectrometry with ZnO QuEChERS |
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| Abstract:A rapid analytical method for the simultaneous determination of 7 lincosamides and macrolides residues in honeys was developed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were dissolved with phosphate buffer(pH 8.0),then extracted with 1% ammonia acetonitrile and salted out with anhydrous sodium sulfate.The extract was cleaned up with 80 mg ZnO and 20 mg PSA.The target compounds were separated on a Waters XBridge C18(150 mm×2.1 mm，5 μm) column with 0.1% formic acid solution and acetonitrile as mobile phases,then determined with electrospray ionization source in positive ion mode under multiple reaction monitoring(MRM) acquisition mode,and quantified by external standard method using matrix matched standard solution.Results showed that the 7 target compounds showed good linearity in their respective mass concentration ranges with correlation coefficients(r) not less than 0.999 3.The limits of detection of the method were in the range of 0.21-0.35 μg/kg,while the limits of quantitation were 0.69-1.16 μg/kg.At three spiked levels of 5.0,10.0 and 20.0 μg/kg,the average recoveries for 7 target compounds were in the range of 75.5%-99.0% with relative standard deviations of 0.78%-5.9%.The method could be applied to the rapid determination of 7 lincosamides and macrolides residues in honeys with the advantages of simplicity,rapidness,high sensitivity and good reproducibility. |
| Key Words:honey high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) lincosamides macrolides zinc oxide(ZnO) QuEChERS |
| 引用本文：杨明，伊鋆，陈丹，王梦颖，许晴，田甜，管卓龙，侯靖，周原，刘坤，王冬梅，胡筱静，卢跃鹏，江小明，涂凤琴.氧化锌QuEChERS/高效液相色谱-串联质谱法测定蜂蜜中7种林可酰胺类与大环内酯类兽药残留[J].分析测试学报,2020,39(8):974-979. |
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