近红外漫反射光谱法快速测定丹参药材中多指标成分的含量

Rapid Determination of Multi-maker Ingredients in Salvia miltiorrhiza by Near Infrared Diffused Reflection Spectroscopy

目的:建立快速测定丹参药材中多指标成分含量的方法。方法:采用高效液相色谱法测定丹参药材中丹酚酸B、迷迭香酸、紫草酸、丹参酮类成分(丹参酮ⅡA+丹参酮Ⅰ+隐丹参酮)的含量(作为参考值)。采用偏最小二乘法-近红外漫反射光谱法建立预测丹参药材中上述指标成分含量的定量模型:根据参考值,采集143批样品,以一阶导数法预处理光谱,丹酚酸B、迷迭香酸、紫草酸、丹参酮类成分的最佳波段分别为6 773.98~3 981.12、6 670.85~3 996.54、8 544.66~3 936.28、8 188.06~3 875.31 cm^(-1)。结果:丹酚酸B、迷迭香酸、紫草酸和丹参酮类成分含量测定方法学验证符合要求。丹酚酸B、迷迭香酸、紫草酸、丹参酮类成分的定量校正模型内部交叉验证相关系数(R^2)分别为0.919 0、0.832 2、0.821 5、0.925 6,校正均方差分别为4.46、0.48、1.34、0.71;外部验证R2分别为0.852 6、0.957 3、0.819 3、0.953 1,均方差分别为9.77、0.28、0.94、0.63。结论:该方法快速、准确、简便、无污染,可用于丹参药材中多指标成分含量的快速测定。

OBJECTIVE：To establish the method for rapid determination of nuezhenoside in Salvia miltiorrhiza. METHODS：The contents of salvianolic acid B,rosmarinic acid,lithospermic acid and tanshinone（tanshinone ⅡA＋tanshinoneⅠ＋cryptotanshinone）were determined by HPLC（as reference value）. Quantitative model for the contents of above components was established by partial least square（PLS）-NIR spectra. According to the reference value,143 samples were collected and the spectrum was pretreated by first-order derivative. The optimal range of wave band for salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were 6 773.98-3 981.12,6 670.85-3 996.54,8 544.66-3 936.28,8 188.06-3 875.31 cm^（-1）. RESULTS：The methodology for the content determination of salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were in line with the requirement. The coefficient（R^2）of internal cross validation for quantitative correction model of salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were 0.919 0,0.832 2,0.821 5,0.925 6. The deviation of corrected mean square roots were 4.46,0.48,1.34,0.71,respectively. The R^2 values of external validation were 0.852 6,0.957 3,0.819 3,0.953 1,respectively;and mean square root of prediction error（RMSEP）were 9.77,0.28,0.94,0.63,respectively. CONCLUSIONS：The method is rapid,accurate,simple and pollution-free,and can be used for rapid determination of multi-maker ingredients in S. miltiorrhiza.