主管:中华人民共和国司法部
主办:司法鉴定科学研究院
ISSN 1671-2072  CN 31-1863/N

›› 2013 ›› Issue (2): 31-34.

• 鉴定实践 • 上一篇    下一篇

超声辅助固相萃取-HPLC法测定不同地区缴获鸦片样品中生物碱

刘翠梅1,白燕平   

  • 收稿日期:2012-11-13 修回日期:2012-12-01 出版日期:2013-03-15 发布日期:2013-04-02
  • 通讯作者: 刘翠梅
  • 基金资助:
    国家科技支撑计划

Determination of Opium Alkaloids by HPLC with Ultrasound-Assisted Solid-Phase Extraction

  • Received:2012-11-13 Revised:2012-12-01 Published:2013-03-15 Online:2013-04-02

摘要: 目的 本文建立了超声辅助固相萃取-HPLC法定量测定缴获鸦片样品中吗啡、可待因、蒂巴因、罂粟碱、那可汀5种生物碱并同时检出6种未知化合物的方法。采用主成分分析法将58份不同地区缴获的鸦片样品分成了4组。方法 采用超声辅助固相萃取法提取生物碱,XDB-C18(5 μm×4.6 mm×250 mm)色谱柱,流动相为10 mM的1-庚烷磺酸钠(pH 3.2)和乙腈,梯度洗脱。结果 该方法的定量限为0.58-2.78 mg/ L。添加水平在0.1-1.5 mg/ mL范围内,平均加标回收率为81%-99.2%,相对标准偏差为1.7%-5.0%。结论 本方法重现性好、定量准确,满足定量检测鸦片中生物碱含量并对不同产地鸦片进行分类的需要。

关键词: 超声辅助固相萃取, 主成分分析, 鸦片, 生物碱, Ultrasound-assisted solid-phase extraction, principle components analysis, opium, alkaloids

Abstract: Objective A novel method for the determination of morphine, codeine, thebaine, papaverine and noscapine together with 6 unknown compounds in seized opium samples by HPLC with ultrasound-assisted solid-phase extraction was established. The principal components analysis (PCA) was used to classify different source opium samples. Methods Ultrasound assisted solid-phase extraction was used to extract alkaloids, and a XDB-C18 column(5 μm×4.6 mm×250 mm)with binary gradients containing 10 mM sodium heptane-1-sulphonate (pH = 3.2) / acetonitrile mixtures was investigated for the analysis. Results LOQ of different alkaloids ranged from 0.58-2.78 mg/ L and recoveries at 0.1-1.5 mg/ mL ranged from 81%-99.2%. RSD% was 1.7%-5.0%. Conclusion This established method can be applied for determining the alkaloids and classifying different source opium samples for its high reproducibility and accuracy.

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