基于安全监管的肾石通颗粒UPLC特征图谱研究

Study on UPLC characteristic spectrum of Shenshitong Granules based on safety supervision

目的建立肾石通颗粒超高效液相色谱(UPLC)特征图谱,并对不同生产企业样品进行初步评价。方法样品采用80%甲醇超声提取,以CAPCELL PAK C_(18)(2.1 mm×150 mm,2μm)为色谱柱,以乙腈-0.1%磷酸溶液作为流动相进行梯度洗脱,流速0.2 mL·min^(-1),柱温35℃,检测波长280 nm,进样量2μL。结果对收集的222批次样品进行分析,通过《中药色谱指纹图谱相似度评价系统》(2012年版)建立了肾石通颗粒超高效液相色谱特征图谱,共确定了15个特征峰,可归属至丹参、牛膝、萹蓄、王不留行、海金沙、鸡内金、瞿麦、金钱草共八味药材,结果表明不同企业间样品相似度差异较大,11批次样品相似度低于0.85,可能存在投料药材质量参差不齐、生产工艺稳定性欠佳等问题。结论该研究建立的特征图谱方法便捷、准确,大幅缩短了分析时间、节约了溶剂,提高了分析效率,为肾石通颗粒质量整体评价提供了依据。

Objective To establish UPLC characteristic spectrum of Shenshitong Granules,and preliminarily evaluate samples from different manufacturers.Methods The sample was extracted by ultrasonic with 80%methanol,a CAPCELL PAK C_(18)(2.1 mm×150 mm,2μm)column was adopted,gradient elution with acetonitrile-0.1%phosphoric acid solution as mobile phase,the flow rate was 0.2 mL·min^(-1),column temperature was 35℃,the detection wavelength was set at 280 nm and injection volume was 2μL.Results The 222 batches of collected samples were injected for analysis,the UPLC characteristic spectrum of Shenshitong Granules was established through the Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine(2012),a total of 15 characteristic peaks hade been identified,which can be attributed to eight medicinal herbs,including Salvia miltiorrhiza Bge.,Achyranthes bidentata Bl.,Polygonum aviculare L.,Vaccaria segetalis(Neck)Garcke,Lygodium japonicum(Thunb.)SW.,Gallus gallus domesticus Brisson,Dianthus superbus L.and Lysimachia christinae Hance.The results showed that the similarity of samples among different enterprises was large,and the similarity of 11 batches of samples was lower than 0.85,there may be problems such as uneven quality of medicinal materials and poor stability of production process.Conclusion The characteristic atlas method established in this study is convenient and accurate,which greatly shortens the analysis time,saves the solvent,improves the analysis efficiency,and provides a basis for the overall evaluation of the quality of Shenshitong Granules.