液相色谱-串联质谱法测定蜂蜜中雷公藤乙素残留量

Determination of the residual concentration of tripdiolide in honey by liquid chromatography-mass spectrometry

目的 建立液相色谱-串联质谱法测定蜂蜜中雷公藤乙素残留量的方法。方法 蜂蜜中雷公藤乙素经乙酸乙酯提取,采用PSA固相萃取小柱净化,用液相色谱-串联质谱进行外标法定量测定。结果 雷公藤乙素在50~1 000 ng/ml范围内线性关系良好(y=1.020 6x-7.830 2,r=0.999 3),检出限为10μg/kg,定量限均为30μg/kg,在30、60、300μg/kg 3个添加水平下加标的平均回收率为70.0%~75.9%,相对标准偏差(RSD)为5.6%~9.2%(n=6)。结论 本方法专属性强,灵敏度高,适用于蜂蜜中雷公藤乙素的残留量定量分析。

Objective To establish a liquid chromatography-mass spectrometry(LC-MS)method for the quantification of residual concentration of tripdiolide in honey.Methods Tripdiolide in honey,a Chinese medicine,was extracted by ethyl acetate and purified by PSA solid phase extraction column,then was quantified by the external LC-MS calibration.Results Good linearities were obtained for tripdiolide in the range of 50-1000 ng/ml(y=1.0206x-7.8302,r=0.9993).The limit of detection was 10μg/kg,and the limit of quantification was all 30μg/kg.The average recoveries at three spiked levels of 30,60 and 300μg/kg ranged from 70.0% to 75.9%,and the relative standard deviation(RSD)was 5.6%-9.2%(n=6).Conclusion The method is highly specific and sensitive,which is applicable to quantitative analysis of residual concentration of tripdiolide in honey.