| 液相色谱-串联质谱测定饲料中溴吡斯的明 |
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| 基金项目:广东省科技计划项目（粤科规财字【2015】110号)；广东省自然科学基金项目（2015A030310184)；畜禽产品农药残留及环境污染物摸底排查与关键控制点评估（GJFP201700704) |
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| 中文摘要:建立了饲料中溴吡斯的明的液相色谱-串联质谱（LC-MS/MS)测定方法。配合饲料、浓缩饲料、精料补充料经甲醇提取，添加剂预混合饲料经乙腈提取后，氮气吹干浓缩，超纯水复溶，采用正己烷脱脂及混合性弱阳离子交换柱（WCX)净化，C18（150 mm ×30 mm，3 μm)色谱柱分离，以乙腈和5 mmol/L甲酸铵为流动相进行梯度洗脱，流速为03 mL/min，柱温为40 ℃。待测物采用电喷雾离子源（ESI)正离子多反应监测（MRM)模式检测，内标法定量。结果表明，不同饲料基质中溴吡斯的明在1~100 μg/L范围内线性关系良好，相关系数（r2)均在0999以上；检出限为10 μg/kg，定量下限为20 μg/kg。饲料中平均回收率为961%~108%，相对标准偏差（RSD)为28%~83%。该方法具有灵敏、准确、重现性好、操作简单等特点，适用于配合饲料、浓缩饲料、预混合饲料以及精料补充料中溴吡斯的明的分析检测。 |
| 中文关键词:液相色谱-串联质谱法（LC-MS/MS) 饲料 溴吡斯的明 |
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| Determination of Pyridostigmine Bromide in Feed Using Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A sensitive liquid chromatography-tandem mass spectrometric（LC-MS/MS) method was developed for the determination of pyridostigmine bromide in feed.The sample was extracted with acetonitrile or methanol，then concentrated to dryness under nitrogen，finally dissolved in water.The extract was purified with n hexane and solid phase extraction（SPE) column，then separated on a C18（150 mm×30 mm，3 μm) column by gradient elution using acetonitrile-5 mmol/L ammonium formate solution as mobile phase at a flow rate of 03 mL/min and a column temperature of 40 ℃.The qualitative analysis was performed with electrospray ionization in positive mode（ESI+) under multiple reaction monitoring（MRM) mode，and the quantitation was carried out by the isotope internal standard method.Results indicated that the calibration curves for pyridostigmine bromide in different feed matrixes showed good linear relationships in the concentration range of 1-100 μg/L with their correlation coefficients all above 0999.The limits of detection and quantitation were 10 μg/kg and 20 μg/kg，respectively.The recoveries ranged from 961% to 108% with relative standard deviations（RSDs) of 28%-83%.The method is sensitive and accurate，and is suitable for the determination of pyridostigmine bromide in compound feed，concentrated feed，additive premix and concentrate supplement. |
| Key Words:liquid chromatography-tandem mass spectrometry（LC-MS/MS) feed pyridostigmine bromide |
| 引用本文：王威利，李亚菲，张展，何绮霞，黄晓梅，苏秋权，丁晨红，林雪贤，殷秋妙，吴维煇.液相色谱-串联质谱测定饲料中溴吡斯的明[J].分析测试学报,2018,37(8):972-976. |
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