摘要
目的使用气相色谱-质谱联用仪(GC-MS)对大黄酚进行解析鉴定,并建立气相色谱-选择监测离子质谱法(GC-MS-SIM)测定大黄中大黄酚的含量。方法大黄酚对照品经乙酸乙酯溶解,以DB-5MS(30m×0.32 mm×0.25μm)石英毛细管柱为色谱柱,全扫描模式下(m/z 50~300 amu)对其主要碎片进行分析,采用蛇床子素为内标,样品经过乙酸乙酯直接提取,选择离子监测法定量分析,监测离子为m/z 254,采用GCMS测定其在大黄中的含量。结果大黄酚主要碎片离子m/z 254(M+),226,225,198,197,180,169,152,141和115,在5~150μg/mL(r=0.9976)范围内线性良好;平均回收率为97.3%,检测限为0.1ng/mL,平均回收率97.3%。结论 GC-MS适用于大黄酚结构解析鉴定,归属了主要碎片途径,所建立的GC-MS-SIM方法简便、快速、灵敏度高、结果准确可靠,可以用于测定大黄中大黄酚的含量。
Objective To develop a gas chromatography-mass spectrometry(GC-MS)method for the characterization of chrysophanol and a GC-MS in single ion monitoring(SIM)method for the determination of chrysophanol in rhubarb. Methods Chrysophanol was dissolved by ethyl acetate and was identified on the DB-5 MS quartz capillary chromatographic column by GC-MS in m/z 50-300 amu full scan mode. Osthole was an internal standard. The sample was extracted by ultrasound in acetic ether and chrysophanol was analyzed quantitatively by elective ion monitoring and selective ion was m/z 254. Results The main fragment ions of chrysophanol were m/z 254(M+),226,225,198,197,180,169,152,141 and 115. There was a good linear relationship in the range of 5~150μg/m L(r=0.9976)for chrysophanol. The average recovery was 97.3% and the detection limit was 0.1 ng/m L. Conclusion It is suitable for determination the fragmentation and investigation of the fagmentation pathways of chrysophanol by GC-MS.The developed GC-MS-SIM method is convenient,rapid,sensitive and suitable for analysis of chrysophanol in rhubarb.
作者
王伟
朱军
陈琴华
WANG Wei;ZHU Jun;CHEN Qinhua(Sinopharm Dongfeng Huaguo Hospital,Shiyan 442000;Medical Laboratory Center,Affiliated Dongfeng Hospital,Hubei University of Medicine,Shiyan 442008;Hubei Key Laboratory of Wudang Local Chinese Medicine Research(Hubei University of Medicine),Shiyan 442000)
出处
《湖北中医药大学学报》
2020年第3期54-57,共4页
Journal of Hubei University of Chinese Medicine
基金
武当特色中药研究湖北省重点实验室(湖北医药学院)开放课题(项目编号:WDCM2018004)
十堰市科技局项目(项目编号:19Y82和19Y115)
