高效毛细管电泳分析法检测中药红曲的桔霉素含量

Determination of citrinin in red kojic by HPCE

目的：建立高效毛细管电泳法测定中药红曲中微量毒性成分桔霉素的方法。方法：采用复合提取剂提取红曲样品，熔融石英毛细管柱50μm×45cm（有效长度40cm）；缓冲体系为20mmol·L^-1硼砂含10mmol·L^-1脱氧胆酸钠（pH9．3），进样压力34．5kPa，分离电压15kV（恒压方式），柱温25℃，检测波长212nm。结果：桔霉素检测的回归方程为Y=9434＋16781X（r=0．990）；最低检测限为0．5mg·mL^-1，相对回收率98．8％～101．1％，日内和日间RSD分别为0．83％～1．54％和1．86～5．09％。结论：本法灵敏准确，简便易行，重现性好，专属性强，可用于中药红曲桔霉素含量的检测。

Objective： To establish an instant determination method of citrinin in red kojic by high performance capillary electrophorphores for the first time. Method： Red kojic was extracted with the mixtrue of Toluene and ethyl acetate （70： 30）. Separation was carried out in an uncoated fused silica capillary （50 μm x45.0 cm）. Meanwhile, a running voltage 15 kV, 20 mmol·L^-1 borax buffer with 10.0 mmol· L^-1 sodium deoxycholate （pH 9. 3） and a UV detector at 212 nm were adopted. Result： Regression equation of citrinin was Y = 9 434 ＋ 16 781X （r = 0. 990）, The lower limit of quantification （S/N ≥3 ） was 0. 5 mg · mL^-1. The assay coefficients of variation ranged from 98.8% to 101.1%. The intra and inter recovery ranged from 0. 83 to 1.54% and from 1.86 to 5.09%. Twenty samples were determined with the method. Conclusion： The method is proved to be simple, rapid and accurate, and it can be used to determine citrinin in red kojic.