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目的:建立快速测定怀地黄中总苯乙醇苷及总环烯醚萜苷含量的方法。方法:采用紫外-可见分光光度法测定药材样品中总苯乙醇苷及总环烯醚萜苷的含量。采用近红外光谱法结合偏最小二乘法,最佳光谱预处理方法分别为多元散射校正法联合一阶导数法、标准归一化法联合一阶导数法,最佳光谱范围分别为6 703.35~11 065.54 cm-1、 3 999.63~9 102.36 cm-1,最佳主因子数分别为10、7,建立药材样品中总苯乙醇苷及总环烯醚萜苷含量的定量分析模型。结果:药材样品中总苯乙醇苷及总环烯醚萜苷含量测定方法学经验证符合要求。总苯乙醇苷、总环烯醚萜苷定量模型的校正集内部交叉验证相关系数分别为0.998 2、0.980 9,校正均方根偏差分别为0.032 7、0.186 0,预测均方根偏差分别为0.035 5、0.035 1,交叉验证均方根偏差分别为0.256 9、0.574 3。总苯乙醇苷、总环烯醚萜苷含量的预测值分别为0.268%~1.636%、3.424%~6.978%,测定值分别为0.299%~1.629%、3.431%~6.952%,绝对偏差分别为-0.042%~0.067%、-0.111%~0.088%,相对偏差分别为-0.819%~0.076%、-2.257%~1.672%,预测值与测定值比较差异均无统计学意义(P>0.05)。结论:该方法快速准确、简便,可用于不同种质怀地黄中总苯乙醇苷及总环烯醚萜苷含量的测定。
OBJECTIVE: To establish a method for rapid determination of total phenylethanoid glycosides and total iridoid glycosides in the root of Rehmannia glutinosa. METHODS: The contents of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples were determined by UV spectrophotometry. Quantitative model of total phenylethanoid glycosides and total iridoid glycosides in medicinal samples was established by NIRS-PLS method. The optimal pretreatment spectra were multivariate scattering correction combined with first derivative method, standard normalization combined with first derivative method. The optimum spectral ranged from 6 703.35-11 065.54 cm-1 and 3 999.63-9 102.36 cm-1. The optimum principal factor number were 10 and 7. RESULTS: The content determination of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples was proved to meet the requirements by methodological experience. The internal cross validation determination coefficients of total phenylethanoid glycosides and total iridoid glycosides were 0.998 2 and 0.980 9. The correction of root mean square error was 0.032 7 and 0.186 0. The root mean square error of prediction were 0.035 5 and 0.035 1. The root mean square error of cross validation were 0.256 9 and 0.574 3. The predicted values of total phenylethanol glycosides and total iridoid glycosides were 0.268%-1.636% and 3.424%-6.978%, respectively; the determination value of them were 0.299%-1.629% and 3.431%-6.952%, respectively; the absolute deviations were -0.042%-0.067% and -0.111%-0.088%, respectively;the relative deviations were -0.819%-0.076%、-2.257%-1.672%, respectively;There was no statistical significance between predicted values and measured values (P>0.05). CONCLUSIONS: The method is accurate and simple. The method can be used for the rapid determination of total phenylethanoid glycosides and total iridoid glycosides in different germplasms of R. glutinosa.
怀地黄近红外光谱法偏最小二乘法总苯乙醇苷总环烯醚萜苷快速测定
Rehmannia glutinosaNIRSPLSTotal phenylethanoid glycosidesTotal iridoid glycosidesRapid determination
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