巴豆苷水解产物异鸟嘌呤测定的方法学研究

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。

Study on the methods for detection of hydrolyzate of crotonoside-isoguanine in stewed soup

Objective To study the method for detection of hydrolyzate of crotonoside - isoguanine in stewed soup. Methods The method of pretreatment includes ultrasonic extraction using aeetonitrile and solution lamination by adding sodium chloride. Then the samples were separated by reverse phase liquid chromatography and detected by mass spectrometer. The interference was eliminated by optimizing the chromatographic conditions. Results Sample handling was very simple and sample processing time was 15 min only. The extraction efficiency was more than 75% and the purification effect was excellent. The method was accurate and showed strong anti-interference ability. The curve fitting was with good linear from 1 to 500 ng/mL, correlation coefficient was 0.9987. The detection limit was 0.5 ng/g and the quantitation limit was 2 ng/g. RSD was 7.6%-11.6%. Conclusion The method developed is simple, reliable and suitable to emergency detection of food poisoning samples.