近红外光谱法快速测定女贞子药材中女贞苷的含量
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篇名: 近红外光谱法快速测定女贞子药材中女贞苷的含量
TITLE:
摘要: 目的:建立快速测定女贞子药材中女贞苷含量的方法。方法:采用高效液相色谱法(HPLC)测定药材中女贞苷的含量(作为参考值):色谱柱为Diamonsil C18,流动相为乙腈-水(梯度洗脱),流速为1.0 ml/min,检测波长为230 nm,柱温为30 ℃,进样量为10 μl。采用偏最小二乘法-近红外光谱法建立预测药材中女贞苷含量的定量校正模型:根据HPLC法含量测定结果,采集校正集样品72份、验证集样品24份,以多元散射校正法联合一阶导数法预处理光谱,最佳波段为9 999.89~4 001.01 cm-1,主成分因子数为9。结果:女贞苷含量测定方法学考察符合要求。女贞苷含量预测的定量校正模型内部交叉验证决定系数为0.984 69,校正均方根偏差为0.097,预测均方根偏差为0.100,交叉验证均方根偏差为0.240 13,预测值与实测值差异无统计学意义(P>0.05)。结论:该方法快速、准确、简便、无破坏、无污染,可用于女贞子药材中女贞苷含量的快速测定。
ABSTRACT: OBJECTIVE: To establish a method for the rapid determination of ligustroflavone in Fructus ligustri. METHODS: HPLC was conducted to determine the content of ligustroflavone (as reference value): the column was Diamonsil C18 with mobile phase of acetonitrile-water (gradient elution) at a flow rate of 1 ml/min, the detection wavelength was 230 nm, column temperature was 30℃ and the injection volume was 10 μl. Partial least square (PLS)-near infrared spectroscopy (NIRS) were adopted to establish the quantitative calibration model of ligustroflavone content: according to the determination results of ligustroflavone content, 72 samples of calibration set and 24 samples of validation set were collected and pretreated spectrum by multivariate scattering correction (MSC) combined with the First Derivative, the optimized wavelength band was 9 999.89-4 001.01 cm-1 and principal component factor number was 9. RESULTS: Methodology validation of content determination for ligustroflavone was in line with the requirement. Internal cross-validation coefficient of the quantitative calibration model for ligustroflavone was 0.984 69, corrected root mean square deviation was 0.097, the root mean square error of predication was 0.100, and the root mean square error of cross validation was 0.240 13. There was no significant different between the predicted value and the measured value. CONCLUSIONS: The method is rapid, accurate, simple without destruction and pollution, and can be used for the rapid determination of ligustroflavone in F. ligustri.
期刊: 2016年第27卷第36期
作者: 张迪文,白雁,谢彩侠,雷敬卫,周琳琳,张苗
AUTHORS: ZHANG Diwen,BAI Yan,XIE Caixia,LEI Jingwei,ZHOU Linlin,ZHANG Miao
关键字: 近红外光谱法;偏最小二乘法;女贞子;女贞苷;含量
KEYWORDS: Near-infrared spectroscopy; Partial least square; Fructus ligustri; Ligustroflavone; Content
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