摘要:
建立了超高效液相色谱-串联质谱法测定保健酒中紫杉醇含量的方法。样品用水稀释10倍后经GCB固相萃取小柱净化,采用LunaC8 100A(150 mm×2 mm,3 μm)柱以0.2%甲酸溶液和乙腈为流动相进行梯度洗脱分离,电喷雾电离(ESI)正离子化和多反应监测模式(MRM)检测。紫杉醇在1~100 μg/L范围内呈良好的线性关系,决定系数(R2)大于0.999,方法的定量限(S/N=10)为10 μg/L;以保健酒为基质,紫杉醇在10.0、50.0和100.0 μg/L 3个水平下的平均加标回收率为88.9%~92.4%,相对标准偏差(RSD,n=6)为7.8%~9.5%;用建立的方法分析了17批实际样品,其中2批次样品有检出,且含量均超过方法定量限的100倍以上。该法简单、高效、灵敏、准确,可用于测定保健酒中紫杉醇的含量,为执法机关监管保健酒里添加红豆杉的违法行为提供了技术支持。
Abstract:
A rapid method for the determination of paclitaxel in health care wine using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed. The sample was diluted with water for 10 times,cleaned up by GCB SPE column,and loaded onto Luna C8(150 mm×2 mm,3 μm)using a mobile phase gradient with 0.2% formic acid and acetonitrile. The determination was carried out with electrospray ion source under the positive(ESI+)and multiple-reaction monitoring(MRM)mode. The calibration curves showed a good linearity in the range of 1~100 μg/L,and the coefficients of determination(R2)were higher than 0.999. The limits of quantification(LOQ,S/N=10)of paclitaxel was 10 μg/L for the health care wine. The average recoveries were from 88.9% to 92.4%,and the relative standard deviation(RSD)was from 7.8% to 9.5% at the spiked levels of 10.0,50.0 and 100.0 μg/L in health care wine(n=6). Seventeen batches of health wine samples were detected using the method,two batches of samples were detected,and the contents were all more than 100 times of the quantitative limit of the method.The method proved to be simple,efficient,sensitive and accurate,and could be used to detect the paclitaxel in health care wine. It would provide technical support for law enforcement agencies to supervise the illegal act of adding Taxus in health wine.
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