HPLC-CAD结合化学计量学的川楝子饮片指纹图谱研究

Chromatographic fingerprint analysis of Toosendan Fructus by HPLC-CAD coupled with chemometrics methods

建立川楝子饮片的高效液相串联电雾式检测器(HPLC-CAD)指纹图谱。采用Agilent ZOBAX SB C_(18)(4.6 mm×250 mm,5μm)色谱柱;以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,柱温30℃,进样量5μL,流速为1mL·min^(-1);CAD雾化气为氮气,雾化气压力为35 psi,雾化室温度35℃。采用相似度评价、聚类分析及主成分分析等方法,对不同来源、不同产地的20批次饮片进行系统比较与归类。结果确定了28个共有峰,并对其中的6个色谱峰进行了指认和鉴定,将不同产地的样品分为3类。方法学考察结果表明,该方法精密度、重复性以及稳定性良好,为市售川楝子饮片的质量评价和控制提供了更加全面科学的依据。

A new method was developed for the chromatographic fingerprint analysis of Toosendan Fructus by HPLC coupled with the charged aerosol detector（CAD） in the present study. Samples were well separated on an Agilent ZOBAX SB C_（18） column（4.6 mm × 250 mm, 5 μm） by gradient elution using acetonitrile and water containing 0.1 % formic acid（v/v） at the flow rate of 1.0 m L·min（-1）. The column temperature was 30 ℃ and the injection volume was 5 μL. The nitrogen inlet pressure of the charged aerosol detector（CAD） was 35 psi, and the nebulizer chamber temperature was 35 ℃. In addition, the method of the chromatographic fingerprints combined with multivariate statistical analysis was effective and reasonable lead to an accurate classification of 20 batches of samples from different locations. The results showed that 28 common peaks were observed in the fingerprint and the samples were classified into three clusters. The established method was well validated, and showed high precision, good repeatability, and satisfactory stability. It may serve in the quality control and evaluation of Toosendan Fructus.