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目的建立HPLC快速测定乌头类生物碱中毒事件中毒患者尿液中乌头碱、次乌头碱、新乌头碱的方法。方法收集乌头碱中毒患者48 h内尿液,经0.1 mol/L HCl酸化,Waters Oasis MCX固相萃取小柱净化,0.5%氨水的甲醇洗脱,氮气吹干,乙腈-10 mmol/L乙酸铵(50∶50,V/V)定容,经Agilent XDB C_8(4.6 mm×250 mm,5.0μm)分离,用紫外检测器,235 nm波长定性定量分析。结果乌头碱中毒患者尿液中乌头碱、次乌头碱、新乌头碱的方法检出限为10μg/L,2个水平的平均回收率为76.0%~115.0%,6次平行测定变异系数(CV)为4.1%~8.2%。在草乌中毒患者的尿液中检出新乌头碱,含量为0.28 mg/L~1.60 mg/L,乌头碱和次乌头碱未检出。结论该方法测定乌头类生物碱中毒事件中毒患者尿样的乌头碱、次乌头碱、新乌头碱方便、快速、准确、可靠、实用性强。
OBJECTIVE To establish a HPLC method for rapid determination of aconitine, hypaconitine and mesaconitine in the urine of patients poisoned by aconitine alkaloids. Methods Urine was collected within 48 hours after aconitine poisoning. The cells were acidified with 0.1 mol / L HCl, cleaned up with Waters Oasis MCX solid phase extraction cartridge, eluted with 0.5% ammonia solution, dried with nitrogen, Ammonium (50:50, V / V) was used to separate and determine by Agilent XDB C_8 (4.6 mm × 250 mm, 5.0 μm). Qualitative and quantitative analysis was performed with a UV detector and a wavelength of 235 nm. Results The detection limit of aconitine, hypaconitine and mesaconitine in urine of aconitine poisoning was 10μg / L, and the average recoveries of two levels were 76.0% ~ 115.0% The coefficient of variation (CV) ranged from 4.1% to 8.2%. The aconitine was detected in the urine of patients with aconite poisoning, the content was 0.28 mg / L ~ 1.60 mg / L, and aconitine and hypaconitine were not detected. Conclusion This method is simple, rapid, accurate, reliable and practical for the determination of aconitine, hypaconitine and mesaconitine in urine of poisoning patients with aconite alkaloid poisoning.