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目的开展熬制汤料中巴豆苷水解产物-异鸟嘌呤测定的方法学研究。方法采用乙腈提取,氯化钠分层的预处理法,液相色谱与串联质谱联用测定异鸟嘌呤;对异鸟嘌呤测定中存在的干扰及消除方法进行了研究。结果乙腈提取与氯化钠分层的预处理法,样本提取时间短(约15min)、效率高(<75%)、操作简单、净化效果好;用液相色谱与串联质谱联用法测定异鸟嘌呤,抗干扰能力强,定性定量准确:在1~500ng/mL范围内,r=0.9987,检出限为0.5ng/g,定量限为2ng/g,RSD为7.6%~11.6%。结论该方法简单可靠,耗时少,能有效去除干扰,非常适合巴豆中毒事件中的应急检测。
Objective To develop a methodological study on the determination of isoguanine, a hydrolyzate of cotinine, in boiled soup. Methods The isoguanine was determined by acetonitrile extraction, sodium chloride pretreatment, liquid chromatography and tandem mass spectrometry. The interference and elimination methods of isoguanine were studied. Results The pretreatment method of acetonitrile extraction and sodium chloride stratification showed that the extraction time was short (about 15 min), the efficiency was high (<75%), the operation was simple and the purifying effect was good. Purine has strong anti-interference ability and qualitative and quantitative accuracy: r = 0.9987 in the range of 1 ~ 500 ng / mL with a detection limit of 0.5 ng / g, a limit of quantification of 2 ng / g and RSD of 7.6% ~ 11.6%. Conclusion The method is simple and reliable, less time-consuming and can effectively remove the interference, which is very suitable for emergency detection in croton poisoning.