液相色谱-串联质谱法测定饲料中的血根碱和白屈菜红碱

Determination of Sanguinarine and Chelerythrine in Feeds by LC-MS/MS

研究旨在建立液相色谱-串联质谱法(LC-MS/MS)检测饲料中血根碱和白屈菜红碱含量的分析方法。饲料样品用15 mL、0.2%盐酸乙腈溶液超声提取2次,每次20 min,提取液使用HLB固相萃取柱净化、微孔滤膜过滤后进行液相色谱-串联质谱法测定,用外标法定量,对检测方法进行验证。结果显示:在质量浓度为1~100 ng/mL范围内其线性相关系数≥0.999,定量限为0.005 mg/kg,回收率为91.9%~101.0%,相对标准偏差为2.00%~7.96%。表明所建立的液相色谱-串联质谱法结果准确、重复性好,适用于饲料中血根碱和白屈菜红碱的测定。

An analytical mehod for the determination of sanguinarine and chelerythrine in feeds by liquid chromatography tandem mass spectrometry(LC-MS/MS)method was established in this experiment.San-guinarine and chelerythrine were extracted twice with 15 mL,0.2%hydrochloric acid acetonitrile solu-tion in ultrasonic water bath for 20 min.The extract was purified by HLB,and filtered through micoron filter,and analyzed by LC-MS/MS.The method was validated.The results showed that the correlation co-efficient was over 0.999 in the range of 1 to 100 ng/mL;the quantitation limit was 0.005 mg/kg;recover-ies were ranged from 91.9%to 101%,and RSD was ranged from 2.00%to 7.96%.This method was accu-rate and suitable to determine sanguinarine and chelerythrine in feeds.