蜂产品中9种硝基咪唑类药物原药及代谢物残留量的HPLC-APCI(+)MS/MS分析
Journal of Instrumental Analysis(2009)
Abstract
运用高效液相色谱-大气压电离串联四极杆质谱(HPLC-APCI(+)MS/MS)内标法分析了蜂蜜、蜂王浆及冻干粉中甲硝唑、地美硝唑(二甲硝唑)、替硝唑、洛硝唑(罗硝唑)、特尼哒唑、异丙硝唑,以及羟基化甲硝咪唑、羟基化异丙硝唑、2-羟甲基-1-甲基化-5-硝咪唑9种硝基咪唑类药物残留量。样品添加氘代标示物HMMNI-D3、IPZ-OH-D3后,用乙腈提取,通过Oasis MCX C18SPE柱净化,Waters Superiorex ODS C18色谱柱分离,采用梯度洗脱,流动相为0.1%甲酸水溶液和0.1%甲酸乙腈溶液,大气压电离源正离子MRM模式检测。蜂蜜和蜂王浆样品的定量下限(LOQ,S/N>10)为0.5μg/kg,冻干粉样品的LOQ为1.0μg/kg。在0.5~50.0μg/L范围内,峰面积与质量浓度呈良好线性,r为0.993 2~0.999 5。
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Key words
nitroimidazole,HPLC-MS/MS,APCI,freeze-dried powder,royal jelly,honey
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