Zhi Xu-Ran, Zhang Zhi-Yong, Jia Pei-Pei, Zhang Xiao-Xu, Yuan Lin, Sheng Ning, Zhang Lan-Tong
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang, Hebei 050017, PR China ; Department of Pharmacy, Hebei General Hospital, Shijiazhuang, Hebei 050051, PR China.
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang, Hebei 050017, PR China.
Pharmacogn Mag. 2015 Jan-Mar;11(41):196-207. doi: 10.4103/0973-1296.149739.
Fructus Sophorae pill, one of the traditional Chinese medicine, was widely used for hemorrhoids, hypertension and odontalgia. This paper describes a sensitive and specific assay for the determination of the 15 active constituents (sophoricoside, genistin, genistein, rutin, quercetin, kaempferol, baicalein, baicalin, naringin, naringenin, hesperidin, neohesperidin, wogonin and cimifugin, prim-O-glucosylcimifugin) in Fructus Sophorae pill.
Chromatographic separation was performed on a C18 column with acidified aqueous methanol gradients at a flow rate of 0.8 mL/min. The identification and quantification of the analytes were achieved by use of a hybrid quadrupole linear ion trap mass spectrometer. Multiple-reaction monitoring scanning was applied to quantification with switching electrospray ion source polarity between positive and negative modes.
The proposed method was used to analyze 40 batches of samples with good linearity (r, 0.9990-0.9999), intraday precisions (RSD, 0.14-2.55%), interday precisions (RSD, 0.51-2.81%), stability (RSD, 0.31-2.65%), and recovery (RSD, 1.29-2.95%) of the 15 compounds. In addition, the hierarchical cluster analysis, including a method called furthest neighbor and nearest neighbor, was employed to classify samples according to characteristics of the 15 constituents.
The results indicated that the analytical method was rapid, reliable, simple and suitable for the quality evaluation of Fructus Sophorae pill.
槐角丸是一种传统中药，广泛用于治疗痔疮、高血压和牙痛。本文描述了一种灵敏且特异的测定槐角丸中15种活性成分（槐角苷、染料木苷、染料木素、芦丁、槲皮素、山柰酚、黄芩素、黄芩苷、柚皮苷、柚皮素、橙皮苷、新橙皮苷、汉黄芩素和升麻素苷、升麻素）的分析方法。
采用C18柱，以酸化甲醇水溶液梯度进行色谱分离，流速为0.8 mL/min。通过使用混合四极杆线性离子阱质谱仪对分析物进行鉴定和定量。采用多反应监测扫描进行定量，在正、负模式之间切换电喷雾离子源极性。
该方法用于分析40批样品，15种化合物具有良好的线性关系（r，0.9990 - 0.9999）、日内精密度（RSD，0.14 - 2.55%）、日间精密度（RSD，0.51 - 2.81%）、稳定性（RSD，0.31 - 2.65%）和回收率（RSD，1.29 - 2.95%）。此外，采用最远邻和最近邻等层次聚类分析方法，根据15种成分的特征对样品进行分类。
结果表明该分析方法快速、可靠、简便，适用于槐角丸的质量评价。
