高效液相色谱-二极管阵列检测器同时测定中药中玉米赤酶烯酮和α-玉米赤霉烯醇  

Simultaneous determination of zearalenone and α-zearalenol in traditional Chinese medicines by HPLC-DAD

作　　者：申红红[1,2] 杨美华[1] 欧阳臻[2] 

机构地区：[1]中国医学科学院药用植物研究所,北京100193 [2]江苏大学药学院,镇江212013

出　　处：《中华中医药杂志》2012年第5期1261-1265,共5页China Journal of Traditional Chinese Medicine and Pharmacy

基　　金：科技部重大新药创制专项(No.2009ZX09502-025);国家中医药管理局2008年度中医药行业科研专项(No.200807042)~~

摘　　要：目的:建立同时测定不同中药中真菌毒素玉米赤酶烯酮(ZON)和α-玉米赤霉烯醇(α-ZOL)的高效液相色谱法,并采用高效液相色谱-串联质谱法(HPLC-ESI-MS/MS)对阳性结果进行确证。方法:样品经甲醇-水溶液(80:20,v/v)提取,免疫亲和柱净化,C18分析色谱柱分离,以水-乙腈(50:50,v/v)为流动相,检测波长236nm,测定结果采用HPLC-ESI-MS/MS进行确证。结果:在0.02-2.50μg/mL范围内,ZON和α-ZOL的线性相关系数均为0.9998。通过添加回收试验,ZON 3个添加水平的回收率为83.8%-98.1%,相对标准偏差为0.9%-7.3%;α-ZOL 3个添加水平的回收率为88.4%-95.5%,相对标准偏差为1.9%-6.2%。ZON和α-ZOL的定量限(S/N=10)分别为18μg/kg和15μg/kg。结论:该方法简便,准确,适用于中药中微量真菌毒素ZON和α-ZOL的检测。Objective： To establish a HPLC method for the simultaneous determination of zearalenone （ZON） and α -zearalenol （ α -ZOL） in traditional Chinese medicines. Methods： The samples were extracted by methanol-water （80：20, v/v）, cleaned up by immunoaffinity column. The HPLC separation was performed on a Cl8 column, and the mobile phase was acetonitrile-water （50：50, v/v）. The detection wavelength was set at 236nm. Positive samples were further confirmed by LC-ESI-MS/MS. Results： The calibration curves showed a good linearity in the range of 0.02-2.501μg/mL, and the correlation coefficients （r） was 0.9998 both of ZON and α-ZOL. The recoveries of ZON were 83.8%-98.1% with the relative standard deviations of 0.9%-7.3%, and the recoveries of α -ZOL were 88.4%-95.5% with the relative standard deviations of 1.9%-6.2%. In the detection of spiked samples, the quantification limit of the method was 181μg/kg and 151μg/kg respectively for ZON and α -ZOL. Conclusion： This method was simple, accurate and reliable for the detection of ZON and α -ZOL in traditional Chinese medicinals.

关 键 词：高效液相色谱-二极管阵列检测器 高效液相色谱-串联质谱法 中药 玉米赤酶烯酮 α-玉米赤霉烯醇 

分 类 号：R284.1[医药卫生—中药学]