快速溶剂萃取-电雾式检测器结合柱后补偿液相色谱在4种中成药黄芪甲苷测定中的应用

Determination of Astragaloside Ⅳ in Four Kinds of Chinese Patent Medicines by ASE-CAD Combined with Column Post Compensation Liquid Chromatography

目的建立一种通过快速溶剂萃取(ASE)提取,使用柱后补偿液相色谱结合电雾式检测器(CAD)测定4种中成药(补中益气丸、通窍鼻炎颗粒、醒脑再造胶囊、玉屏风颗粒)中黄芪甲苷含量的方法,并将该方法与药典方法进行差异分析。方法通过试验确定ASE萃取最优条件:水饱和正丁醇作为溶剂,萃取温度100℃,萃取时间5 min,循环次数3次,HPLC方法:色谱柱Thermo AQ-C_(18)(2.1 mm×100 mm,3μm),分析泵流动相:乙腈-水(15∶85),梯度程序:0 min,15%A,0~4 min,15%~60%A,4~5 min 60%A,流速:0.3 mL·min^(-1);补偿泵流动相:乙腈,流速:0.3 mL·min^(-1)。结果黄芪甲苷在26.62~665.5μg·mL^(-1)内呈良好的线性,样品测定RSD为1.0%~2.1%,方法回收率为98.80%~100.80%,方法结果与药典方法结果吻合。结论该方法快速、准确、通用性高、重现性好,可用于这4种中成药中黄芪甲苷的含量测定。

OBJECTIVE To establish a method for determination of astragaloside IV in 4 Chinese patent medicines （ BuZhong YiQi Pills, TongQiao BiYan Granules, XingNao ZaiZao Capsules, YuPing Feng Granules） by accelerate solvent extraction （ASE） combined with column post compensation liquid chromatography and charged aerosol detector （CAD） detection, and compare the result with that of the pharmacopoeia method. METHODS The optimal extraction conditions were determined by the ASE test ：water satu- rated n-butanol was used as solvent, ASE extraction temperature was 100 ℃, extraction time was 7 min and cycle time was 3. For the HPLC analysis, Thermo AQ-C18 column （2. 1 mm x 100 mm,3 μm） was employed, the mobile phase for the analysis pump was com- posed of acetonitrile-water （ 15： 85） , and the flow rate was 0. 3 mL · min- 1. Gradient program was as follows：0 rain, 15% A; 0 - 4 rain, 15% -60% A; 4 -5 rain 60% A. The mobile phase for the compensating pump was acetonitrile, and the flow rate was 0. 3 mL · min - 1. RESULTS The linear range of the calibration curve of astragaloside IV was 26. 62 - 665.5 μg · mL - 1. The RSD of sample analysis was 1.0% - 2.1%. The average recoveries were 98.80% - 100. 80%. The method is in good agreement with the Pharmacopoeia method. CONCLUSION The method is rapid, accurate and reproducible. It can be used for the determination of as- tragaloside IV in 4 kinds of Chinese patent medicines.