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当前位置: 首页 > 文章 > 猪可食性组织中加米霉素残留量的UPLC-MS/MS检测方法研究 畜牧与兽医 2017 (6) 54-59
Position: Home > Articles > Development of anultra-performance liquid chromatography-tandem mass spectrometry method for the determination of gamithromycin in edible swine tissues Animal Husbandry & Veterinary Medicine 2017 (6) 54-59

猪可食性组织中加米霉素残留量的UPLC-MS/MS检测方法研究

作  者：
郭洋洋;罗小清;彭麟;安冉;吴峰;郭凡溪;余祖功
单  位：
南京农业大学动物医学院
关键词：
加米霉素;猪可食性组织;UPLC-MS/MS;残留检测
摘  要：
建立一种可靠、快速、灵敏的超高效液相色谱-串联质谱法(UPLC-MS/MS)用于猪可食性组织中加米霉素残留量的检测方法。猪可食性组织(肌肉、皮脂、肝脏、肾脏)经绞碎、均质后,用乙腈提取,MCX固相萃取柱净化,Acquity UPLC BEH C_(18)色谱柱梯度洗脱,在电喷雾正离子(ESI+)下选用多反应监测(MRM)模式进行待测物的分析,内标法定量。该方法的检测限(LOD)与定量限(LOQ)分别为2μg·kg~(-1)和5μg·kg~(-1);待测物加米霉素在2~600μg·kg~(-1)的浓度范围内,峰面积与浓度呈良好的线性关系(r2>0.99);加米霉素在猪肌肉、皮脂、肝脏、肾脏组织中的添加回收率为86.8%~107.4%,日内精密度及日间精密度<16.5%。本研究建立了猪可食性组织中加米霉素残留量检测的制样和超高效液相色谱-串联质谱检测方法,适用于猪可食性组织中加米霉素残留量的测定。
译  名：
Development of anultra-performance liquid chromatography-tandem mass spectrometry method for the determination of gamithromycin in edible swine tissues
作  者：
GUO Yangyang;LUO Xiaoqing;PENG Lin;AN Ran;WU Feng;GU Fanxi;YU Zugong;College of veterinary Medicine,Nanjing Agricultural University;
关键词：
gamithromycin;;UPLC-MS/MS;;residues
摘  要：
To establish a reliable,rapid and sensitive method for determination of gamithromycin residues in swine tissues( muscle,skin+fat,liver,kidney),ultra-performance liquid chromatography-tandem mass spectrometry( UPLC-S/MS) was developed and optimized. The samples were extracted with acetonitrile,and then purified via an Oasis MCX solid-phase extraction cartridge. Chromatographic separation was performed on an Acquity UPLC BEH C_(18) column. Analysis was carried out on UPLC-ESI-MS/MS working with multiple reaction monitoring mode. Internal standard was used for quantitation of target drug. The method has a good linearity at the range of 2 ~ 600 μg kg~(-1),with related coefficient of 0. 99. Recoveries of spiked samples ranged from 86. 8% to 107. 4% with relative standard deviation( RSD) less than 16. 5%. The limits of detection( LODs) and quantification( LOQs) were 2 and 5 μg kg~(-1),respectively. The results showed that the pretreatment and purification process established by this study is easy to operate. The method has good stability,reproducibility,sensitivity,and great accuracy.

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