法医学杂志 ›› 2002, Vol. 0 ›› Issue (2): 89-91.

• 论文 • 上一篇    下一篇

柱切换HPLC法分析尿中吗啡和O~6-单乙酰吗啡的研究

张玉荣,汪蓉,张成功,孙志清,王跨陡,刘琦   

  1. 上海市刑事科学技术研究所,上海市刑事科学技术研究所,上海市刑事科学技术研究所,上海市刑事科学技术研究所,上海市刑事科学技术研究所,上海市刑事科学技术研究所 上海200083 ,上海200083 ,上海200083 ,上海200083 ,上海200083 ,上海200083
  • 发布日期:2002-04-25 出版日期:2002-04-28

Column-switching high-performance liquid chromatographic method for the determination of morphine and O~6 -monoacetylmorphine in urine

ZHANGYU-RONG,WANGRONG,ZHANGCHENG-GONG,ETAL.(SHANGHAIINSTITUTE OFFORENSIC SCIENCE,SHANGHAI200083)   

  • Online:2002-04-25 Published:2002-04-28

摘要: 目的建立用柱切换HPLC技术分析尿中吗啡和O6-单乙酰吗啡的方法。方法尿样用硼砂缓冲液(pH9.2)稀释后进入预处理柱(YWG-C18,33mm×5.0mm熏10μm),用H2O洗去杂质,再用CH3OH∶H2O(60∶40)将被分析组分洗脱进入分析柱(LichrospherR100CN,125mm×4.0mm熏5μm),分析流动相为CH3OH∶磷酸盐缓冲液(pH6.86)=22∶78。紫外检测器波长为286nm。结果尿中吗啡和O6-单乙酰吗啡的线性范围分别为50~1600ng/ml和100~1600ng/ml。吗啡和O6-单乙酰吗啡的精密度均小于4%。吗啡和O6-单乙酰吗啡的检测限均为40ng/ml。结论用CSHPLC测定尿中吗啡和O6-单乙酰吗啡,方法准确、灵敏、快速、简便

关键词: 吗啡, O6-单乙酰吗啡, CSHPLC, 尿

Abstract: Objective To develop a column-switching high-performance liquid chromatographic method for the determination of morphine and O 6 -monoacetylmorphine in urine.Methods Urine samples1.0mlwere spiked with1.0ml borate buffer,after centrifugation,1.0ml of supernate were injected directly into an extraction columnYWG C 18 33mm×5.0mm,10 μ m.After a washing step with the extraction mobile phase,the retained morphine and O 6 -monoacetylmorphine were flushed into the analytical columnLichrospher R 100CN125mm×4.0mm,5 μ mwith the mobile phase CH 3 OH-H 2 O60∶40.The analytical mobile phase is CH 3 OH-phosphate bufferpH6.8622∶78.The UV detector was set at λ 286nm.Results The method shows excellent linearity from50to1600ng/ml for morphine and from100to1600ng/ml for O 6 -monoacetylmorphine.The linear correlation coefficients were>0.999.The relative standard deviations were<4%.The limits of detection were40ng/ml for both morphine and O 6 -monoacetylmorphine.Conclusion The method described is sensitive,rapid,reproducible,and simple.

Key words: morphine, O 6-monoacetylmorphine, CSHPLC, urine