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目的建立超高效液相色谱法同时测定胃内容物(或呕吐物)中乌头碱、次乌头碱、新乌头碱的方法。方法样品经0.1 mol/L盐酸提取,8 000 r/min离心20 min,残渣重复提取一次,合并上清液用Oasis HLB固相萃取柱净化后,解析液45℃氮吹至干,已腈-0.1%乙酸(1∶1,V/V)复溶,过0.22μm滤膜进样,ACQUITY UPLC HSS T3柱(2.1 mm×100 mm,1.8μm)液相色谱柱分离,紫外检测器检测,外标法定量。结果乌头碱、次乌头碱、新乌头碱在相应的浓度范围内线性关系良好,相关系数(r)为0.996~0.999 5,检出限分别为0.075 mg/kg、0.10 mg/kg、0.05 mg/kg,定量限分别为0.23 mg/kg、0.30 mg/kg、0.15 mg/kg;空白基质中加标实验显示加标回收率为86.3%~110.9%,加标回收率的精密度为3.50%~9.70%。结论该方法操作简便,准确度好,精密度高,能对胃内容物(或呕吐物)中乌头碱、次乌头碱、新乌头碱进行定性定量检测。
Objective To establish a method for simultaneous determination of aconitine, hypaconitine and mesaconitine in gastric contents (or vomitus) by ultra performance liquid chromatography. Methods The sample was extracted with 0.1 mol / L hydrochloric acid and centrifuged at 8 000 r / min for 20 min. The residue was extracted once. The supernatant was purified with Oasis HLB solid phase extraction column. 0.1% acetic acid (1: 1, V / V), 0.22 μm filter, ACQUITY UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm) liquid chromatographic column was used to detect UV detector Standard method of quantitative. Results The correlation coefficients (r) ranged from 0.996 to 0.999 5 for aconitine, hypaconitine and mesaconitine in the corresponding concentrations. The detection limits were 0.075 mg / kg and 0.10 mg / kg, respectively. 0.05 mg / kg and the limit of quantification were 0.23 mg / kg, 0.30 mg / kg and 0.15 mg / kg, respectively. The spiked recoveries of blank matrix were 86.3% -110.9% 3.50% ~ 9.70%. Conclusion The method is simple, accurate, and accurate. It can qualitatively and quantitatively detect aconitine, hypaconitine and mesaconitine in gastric contents (or vomitus).