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

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。采用主成分分析法区分不同地区缴获的鸦片样品。方法采用超声辅助固相萃取法提取生物碱,XDB-C18（5μm×4.6mm×250mm）色谱柱,流动相为10mM的1-庚烷磺酸钠（pH 3.2）和乙腈,梯度洗脱,紫外检测器检测。结果该方法的定量限为0.58~2.78 mg/kg。添加水平在0.2～1.5mg/mL范围内,平均加标回收率为81.0%～99.2%,相对标准偏差为1.6%～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。

Determination of Opium Alkaloids by HPLC with Ultrasound Assisted Solid Phase Extraction and Its Application in Source Identification

Objective To develop a rapid and reliable method for simultaneous determination of morphine, codeine, thebaine, papaverine, noscapine and 6 other unknown compounds in seized opium samples by high performance liquid chromatography with ultrasonic assisted solid phase extraction. Method Uhrasonic assisted solid phase extraction was used to extract alkaloids. Target analytes were separated on a XDB-C18 column （5 μm×4.6 minx250 mm）, and were gradiently eluted with the binary mobile phase containing 10 mM sodium heptane-l-sulphonate （pH3.2） and aeetonitrile. Results LOQ of different alkaloids ranged from 0.58 to 2.78 mg/mL. Recoveries at 0.2-1.5 mg/mL ranged from 81.0%-99.2% and RSD% was 1.6%-5.0%. The PCA divided 58 seized samples into 4 groups. Conclusion The established method is of high reproducibility and accuracy. It can be applied to determining the alkaloids in opium samples and discriminating different sources of opium.