| 液相色谱-串联质谱法测定蜂蜜中9种青霉素 |
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| 引用本文： | 李学民,母健,王蕾,曹彦忠,张进杰. 液相色谱-串联质谱法测定蜂蜜中9种青霉素[J]. 河北大学学报(自然科学版), 2012, 32(5): 492-498 |
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| 作者姓名： | 李学民 母健 王蕾 曹彦忠 张进杰 |
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| 作者单位： | 秦皇岛出入境检验检疫局,河北秦皇岛,066004 |
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| 基金项目： | 国家标准研制资助项目(20040032-T-442) |
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| 摘 要： | 建立了用液相色谱-串联质谱(LC-MS-MS)测定蜂蜜中9种青霉素残留量的分析方法.3g蜂蜜样品用25mL pH=8.5的0.15mol/L磷酸二氢钠缓冲溶液溶解,用Oasis HLB固相萃取柱净化,目标物用乙腈-水(体积比1∶1)洗脱,定容收集液至3mL.采用电喷雾电离,正离子扫描,多反应监测(MRM)模式检测.0.5,1.0,2.0,5.0μg/kg 4个添加水平的回收率为76.9%～104.3%;相对标准偏差为3.29%～9.12%;方法定量限是:青霉素G、乙氧萘青霉素为0.5μg/kg,氧哌嗪青霉素、青霉素V、苯唑青霉素为1.0μg/kg,羟氨苄青霉素、氨苄青霉素、邻氯青霉素、双氯青霉素为2.0μg/kg.
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| 关 键 词： | 液相色谱-串联质谱 蜂蜜 9种青霉素 |
Determination of 9 penicillins in honey by high-performance liquid chromatography-tandem mass spectrometry |
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| LI Xuemin , MU Jian , WANG Lei , CAO Yanzhong , ZHANG Jinjie. Determination of 9 penicillins in honey by high-performance liquid chromatography-tandem mass spectrometry[J]. Journal of Hebei University (Natural Science Edition), 2012, 32(5): 492-498 |
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| Authors: | LI Xuemin MU Jian WANG Lei CAO Yanzhong ZHANG Jinjie |
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| Affiliation: | (Qinhuangdao Entry-Exit Inspection and Quarantine Bureau,Qinhuangdao 066004,China) |
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| Abstract: | A method was described for the determination of 9 penicillins in honey by LC-MS-MS.3.0 g honey samples were dissolved in 25 mL sodium dihydrogen phosphate buffer solution(pH=8.5),and then cleaned up with Oasis HLB SPE cartridge.The target compounds were eluted with acetonitrile-water(1∶1),and the elution was determined to a volume of 3 mL.MS detection was performed in the positive ion mode using multiple reaction monitoring(MRM).Limit of quantification(LOQ) for the method of 9 penicillins was between 0.5-2.0 μg/kg.Average recoveries at four fortification levels(0.5,1.0,2.0,5.0 μg/kg) in honey were 76.9%-104.3%,relative standard deviation were 3.29%-9.12%. |
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| Keywords: | LC-MS-MS honey 9 penicillins |
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