目的 利用HPLC-電霧式檢測器（charged aerosol detector，CAD）聯(lián)用技術(shù)建立知母中知母皂苷BⅡ和菝葜皂苷元的測定方法，并比較知母鹽制前后兩種成分的變化。方法 知母皂苷BⅡ以乙腈-水（25：75）為流動(dòng)相，進(jìn)樣量為10 μL；菝葜皂苷元以甲醇-水（95：5）為流動(dòng)相，進(jìn)樣量為20 μL；其他色譜條件均采用Thermo C₁₈柱（250 mm×4.6 mm，5 μm），體積流量為1 mL/min，柱溫為30℃；Corona參數(shù)：氮?dú)鈮毫?41.3 kPa，F(xiàn)ilter：High，Range：200 pA。結(jié)果 知母皂苷BⅡ在0.305～4.880 μg線性關(guān)系良好，r=0.999 4，平均回收率為99.1%，RSD值為1.2%；菝葜皂苷元在0.490～7.840 μg線性關(guān)系良好，r=0.999 1，平均回收率為98.0%，RSD值為1.3%。知母中知母皂苷BⅡ?yàn)?.16%～5.92%，鹽制后為4.15%～7.20%；知母中菝葜皂苷元為0.42%～1.39%，鹽制后為0.52%～1.54%。結(jié)論 CAD檢測器具有較為平穩(wěn)的基線和較高的靈敏度，更加適用于知母皂苷類及含有較弱或無紫外吸收成分的測定，知母鹽制后知母皂苷BⅡ和菝葜皂苷元的量均有所升高。

Objective To establish a method for the determination of timosaponin BⅡ and sarsasapogenin in Anemarrhenae Rhizoma by HPLC with the charged aerosol detector (CAD), and to compare the contents of the two components in Anemarrhenae Rhizoma before and after processing with salt-water. Methods Analysis was performed on Thermo C₁₈ column (250 mm×4.6 mm, 5 μm). Acetonitrile-water (25:75) was as the mobile phase for timosaponin BⅡ with the injection volume of 10 μL, and methanol-water (95:5) as the mobile phase for sarsasapogenin with injection volume of 20 μL. The other chromatographic conditions were : flow rate of 1 mL/min and column temperature of 30℃. The Corona parameters were as follows: nitrogen pressure was 241.3 kPa, high filter, and range of 200 pA. Results The linear range of timosaponin BⅡ was 0.305-4.880 μg (r=0.999 4), and the average recovery rate was 99.1% (RSD=1.2%). The linear range of sarsasapogenin was 0.490-7.840 μg (r =0.999 1), and the average recovery rate was 98% (RSD=1.3%). The contents of timosaponin BII were obtained over 3.16%-5.92% for Anemarrhenae Rhizoma and 4.15%-7.20% after processing; The contents of sarsasapogenin were obtained over 0.42%-1.39% for Anemarrhenae Rhizoma and 0.52%-1.54% after processing. Conclusion CAD has some advantages in saponins detection of Anemarrhenae Rhizoma such as its steady baseline and good sensitivity. CAD is the most favorable detector for the determination of saponins or other constituents without UV absorption, and the contents of timosaponin BⅡ and sarsasapogenin increase after processing.

國家自然科學(xué)基金資助項(xiàng)目（81102810）；教育部高等學(xué)校博士學(xué)科點(diǎn)專項(xiàng)科研基金資助項(xiàng)目（20012133120009）