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目的开展熬制汤料中巴豆苷测定的方法学研究。方法采用乙腈提取、氯化钠分层的预处理方法,液相色谱与质谱、光谱联用法测定巴豆苷。通过优化色谱条件,更换检测器排除鸟苷的干扰。结果采用乙腈提取与氯化钠分层的预处理办法,样本提取时间短、效率高、操作简单,并且净化效果好;液相色谱与质谱、光谱联用法测定巴豆苷的抗干扰能力强,定性、定量准确。该方法在1 ng/ml~1 000 ng/ml,质谱测定的线性关系良好,线性相关系数为0.9985;在浓度为1μg/ml~100μg/ml时,紫外-可见光谱测定的线性关系良好,线性相关系数为0.9993。巴豆苷质谱测定的检出限为0.1 ng/g,紫外-可见光谱测定的检出限为0.1μg/g。结论乙腈提取,氯化钠分层预处理,结合液相色谱与质谱、光谱联用法测定熬制汤料中的巴豆苷,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 the cotatins in boiled soup. Methods Pretreatment of acetonitrile extraction, sodium chloride layering, liquid chromatography and mass spectrometry, spectrophotometry for the determination of. By optimizing the chromatographic conditions, the detector was replaced to exclude guanosine interference. Results The pretreatment method of acetonitrile extraction and sodium chloride delamination showed that the extraction time was short, the efficiency was high, the operation was simple, and the purification effect was good. The anti-interference ability of the saponin was determined by liquid chromatography, mass spectrometry and spectrometry. , Quantitative and accurate. The linearity of the method was good at 1 ng / ml ~ 1 000 ng / ml, with a linear correlation coefficient of 0.9985. The linearity of the method was good at 1 μg / ml ~ 100 μg / ml, and the linearity The correlation coefficient is 0.9993. The detection limit of mass spectrometry was 0.1 ng / g, and the detection limit of UV-Vis was 0.1 μg / g. Conclusion Acetonitrile extraction and sodium chloride pretreatment combined with LC-MS and SPECT spectrophotometry for the determination of cotinine in boiled soups are simple and reliable, less time-consuming and effective in removing interferences and are very suitable for croton poisoning In the emergency test.