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塔拉粉酶解废液HPLC指纹图谱及2个主成分含量测定方法研究

HPLC Fingerprint and Content Determination of Two Principal Components in Waste Liquid of Tara Enzymatic Hydrolysis

  • 摘要: 建立了一种同时分析塔拉粉酶解废液中奎宁酸(QA)与没食子酸(GA)的HPLC方法,并进行方法学验证,进一步绘制其HPLC指纹图谱,结合相似度、聚类分析等手段对不同批次塔拉粉酶解废液进行评价。研究结果表明:该方法选择215 nm、流动相乙腈-0.1%三氟乙酸水溶液、乙腈梯度5%~20%、流速1.0 mL/min、柱温30 ℃作为奎宁酸与没食子酸的色谱分析条件;奎宁酸标准曲线线性范围为1.25~20 g/L、其检测限为0.5 g/L,没食子酸标准曲线线性范围为0.062 5~1 g/L、其检测限为5 mg/L;该方法精密度、重复性、稳定性、加样回收试验的RSD均小于5%;奎宁酸与没食子酸平均加样回收率分别为100.87%、99.65%;12批次废液试样指纹图谱分析相似度均大于0.95;可通过聚类分析分为两类,10号和11号样品聚为一类,其余样品聚为一类;计算得到奎宁酸质量浓度为482.3 g/L,没食子酸质量浓度为35.7 g/L。

     

    Abstract: An HPLC method was developed for the simultaneous analysis of quinic acid(QA) and gallic acid(GA) in tara powder enzymatic digestion waste solution, and the methodological verification was carried out. The HPLC fingerprints were further drawn and the different batches of tara powder enzymatic digestion waste solution were evaluated by combining similarity and cluster analysis. The results showed that the detection wavelength at 215 nm, mobile phase acetonitrile-0.1% aqueous trifluoroacetic acid aqueous solution, acetonitrile gradient of 5%-20%, flow rate of 1.0 mL/min and column temperature of 30 ℃ were selected as the chromatographic analysis conditions for quinic acid and gallic acid. The linear range of quinic acid standard curve was 1.25-20 g/L, and the detection limit was 0.5 g/L. The linear range of gallic acid standard curve was 0.062 5-1 g/L, and the detection limit was 5 mg/L. The RSD of precision, repeatability, stability, and the spiked recovery test were less than 5%.The average spiked recoveries of quinic acid and gallic acid were 100.87% and 99.65%, respectively. The similarity of the fingerprint profiles of the 12 batches of waste samples was greater than 0.95. The samples could be divided into two categories by cluster analysis, with samples No.10 and No.11 were clustered into one category, and the rest samples were clustered into one category. The mass concentrations of quinic acid and gallic acid were calculated to be 482.3 g/L and 35.7 g/L, respectively.

     

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