液相色谱-串联质谱法测定血液和尿液中秋水仙碱

发布时间：2018-06-29 08:41

本文选题：法医毒物分析 + 液相色谱-串联质谱法(LC-MS-MS)　；参考：《中国法医学杂志》2009年01期

【摘要】：目的建立检测血液和尿液中秋水仙碱的液相色谱-串联质谱法。方法0.5mL血液或尿液以丁丙诺啡为内标,经pH9.2硼酸盐缓冲溶液碱化后,用乙酸乙酯进行提取,在ZORBAX SB-C18液相柱(150mm×2.1mm×5μm)上以V(甲醇)∶V(20mmol/L乙酸铵和0.1%甲酸缓冲溶液)=80∶20为流动相,流速为0.2mL/min,采用电喷雾正离子模式离子化、多反应监测模式检测秋水仙碱,内标法定量。结果血液、尿液中秋水仙碱与内标丁丙诺啡色谱分离良好,秋水仙碱在0.1~50 ng/mL内均具有良好的线性,相关系数0.9990,最低检出限为0.05ng/mL,方法回收率为94%~116%,日内与日间精密度(RSD)均小于8.5%。结论所建LC-MS-MS方法灵敏度高、操作简便、快速、准确,适用于血液及尿液等生物检材中痕量秋水仙碱成分的检测。
[Abstract]:Objective to establish a liquid chromatography-tandem mass spectrometry method for the determination of colchicine in blood and urine. Methods 0.5 mL blood or urine was alkalized with buprenorphine and alkalized with borate buffer solution at pH 9.2, then extracted with ethyl acetate. The mobile phase was V (methanol): v (20 mmol / L ammonium acetate and 0.1% formic acid buffer solution) on ZORBAX SB-C18 liquid column (150mm 脳 2.1mm 脳 5 渭 m). The flow rate was 0.2mL / min. Colchicine was detected by electrospray ion mode ionization and multi-reaction monitoring mode. The quantity of colchicine was determined by internal standard method. Results Colchicine and buprenolone endorphin in blood and urine were separated well. Colchicine had a good linearity in 0.1 渭 g / mL, the correlation coefficient was 0.9990, the detection limit was 0.05ng / mL, the recovery rate was 940.116, and the precision (RSD) was less than 8.5g / mL. Conclusion the established LC-MS-MS method has the advantages of high sensitivity, simple, rapid and accurate operation. It is suitable for the determination of colchicine in blood and urine.
【作者单位】：复旦大学上海医学院法医学系;司法部司法鉴定科学技术研究所上海市法医学重点实验室;
【基金】：中央级公益性科研院所科研专项基金资助项目(GY0702) 上海市科委资助项目(072512019)
【分类号】：D919

【参考文献】