新生化颗粒的HPLC指纹图谱研究

HPLC characteristic fingerprints of Xinshenghua Keli

新生化颗粒被誉为"产后第一方",在妇科用药领域需求量大,而市场上制剂的质量参差不齐,无法保证临床疗效。为此,采用高效液相色谱建立新生化颗粒指纹图谱,为提高并建立其质量控制标准提供方法。采用Agilent 5 HC-C18(2)(4.6mm×250 mm,5μm)色谱柱进行检测,以甲醇-0.1%甲酸溶液为流动相,梯度洗脱,流速为1 mL·min^-1,进样量为10μL,检测波长为光电二极管阵列检测器(PDA)210.0400.0 nm的最大值,柱温为25℃。建立12批新生化颗粒优质产品的指纹图谱,确定了43个共有峰,并对其及江苏融昱药业10批普通产品、10批不同产家产品进行相似度评价;通过对制剂和各组方药味的保留时间和紫外吸收光谱,及液质联用技术(HPLC-MS)进行比对,对共有峰进行了制剂-药材的来源归属和指认。经方法学验证所建立的新生化颗粒指纹图谱,具有良好的精密度、稳定性和重复性,可用于新生化颗粒的质量综合评价。

Xinshenghua Keli is known as the " preferred prescription of postpartum",with large demand in the field of gynecologic medicine. However,the quality of the preparation is uneven in the market,so its clinical efficacy cannot be guaranteed. In order to improve and establish its quality control standard,high performance liquid chromatography( HPLC) was used to establish the fingerprint of Xinshenghua Keli. The detection was performed on Agilent 5 HC-C18( 2) column( 4. 6 mm × 250 mm,5 microns) with methanol-0. 1% formic acid solution as mobile phase for gradient elution,at a flow rate of 1 mL·min^-1 with column temperature of 25 ℃.The injection volume was 10 μL and detection wavelength was set at the maximum value between 210. 0 nm and 400. 0 nm by Photo-Diode Array( PDA) detector. The fingerprint of 12 batches of high-quality Xinshenghua Keli was established and 43 common peaks were identified. The similarities of crowned products,10 batches of ordinary ones made by Jiangsu Rongyu Pharmaceutical and 10 batches produced by different manufacturers were evaluated. The composition identification and source analysis for the common peaks were performed by comparing the retention time of herbal medicines and ultraviolet absorption spectrum,along with high performance liquid chromatographymass spectrometry( HPLC-MS) technology. The established fingerprint of Xinshenghua Keli,has proven to have good precision,stability and repeatability through the methodology validation,so it can be used to comprehensively evaluate the quality of Xinshenghua Keli.