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固相萃取/高效液相色谱-串联质谱法测定植物性食品中链霉素与双氢链霉素
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作者单位
李敏青,徐娟,王岚,安文佳,孙灵慧,何曼莉 1.广州海关技术中心2.广东省动植物与食品进出口技术措施研究重点实验室 
基金项目:上海市科学技术委员会项目(15ZR1437700);国家中医药管理局(国家中药标准化项目ZYBZH-C-GX-09);国家药典委员会项目(ZG2016-2);广西壮族自治区科学技术厅重大专项计划(2015AC05038);上海市科学技术委员会扬帆计划项目(16YF1410200)
中文摘要:建立了植物性食品(苹果、芹菜、甜椒、干扁豆)中链霉素(Streptomycin,STR)和双氢链霉素(Dihydrostreptomycin,DHS)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经磷酸盐缓冲溶液提取,借助WCX固相萃取柱富集净化后,采用Atlantis Hilic Silica亲水作用色谱柱(100 mm×30 mm,3 μm)分离,乙腈-01 mol/L甲酸铵和01%甲酸溶液等度洗脱,以电喷雾电离串联质谱多反应监测(MRM)正离子模式进行检测,外标法定量。结果显示,链霉素和双氢链霉素在10~120 μg/L质量浓度范围内线性良好,相关系数(r)均大于0999,定量下限均为125 μg/kg。本底空白的4种样品基质在3个添加水平(125、250、500 μg/kg)下的平均回收率为836%~101%,相对标准偏差为23%~78%。该方法无需使用对LC-MS联用仪造成污染的离子对试剂,且方法操作简便、快速、可靠、稳定,能满足大部分植物性食品中链霉素和双氢链霉素的检测需要。
中文关键词:植物性食品  链霉素  双氢链霉素  高效液相色谱-串联质谱(HPLC-MS/MS)
 
Determination of Streptomycin and Dihydrostreptomycin in Vegetable Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction
Abstract:A method was established for the determination of streptomycin(STR) and dihydrostreptomycin(DHS) in vegetable foods(apple,celery,capsicum and lentil) based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The sample was extracted with phosphate buffer and cleaned up with a WCX solid phase extraction cartridge.The extracts were separated on an Atlantis Hilic Silica column(100 mm×30 mm,3 μm) using acetonitrile-01 mol/L ammonium formate and 01% formic acid as mobile phases by isocratic elution,then detected by HPLC-MS/MS in positive ion mode under multiple reaction monitoring(MRM) mode.An external standard method was used for quantitative analysis.The calibration curves for streptomycin and dihydrostreptomycin showed good linearity in the range of 10-120 μg/L with their correlation coefficients(r) more than 0999.The limits of quantitation(LOQs) were both 125 μg/kg.The average recoveries for streptomycin and dihydrostreptomycin at three spiked levels of 125,250 and 500 μg/kg ranged from 836% to 101%,with the relative standard deviations(RSDs) of 23%-76%.With no need of ion pair reagents resulting in the contamination of liquid chromatography-mass spectrometer,the method is simple,rapid,reliable and stable,and could meet the requirements for determination of streptomycin and dihydrostreptomycin residues in most vegetative samples.
Key Words:vegetable foods  streptomycin  dihydrostreptomycin  HPLC-MS/MS
引用本文:李敏青,徐娟,王岚,安文佳,孙灵慧,何曼莉.固相萃取/高效液相色谱-串联质谱法测定植物性食品中链霉素与双氢链霉素[J].分析测试学报,2019,(7):859-864.
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