目的:建立氢核磁定量方法测定何首乌及其炮制品中大黄素和大黄素甲醚的含量。方法:以氘代二甲基亚砜为测试溶剂,以顺丁烯二酸(δH6.25)为内标物,以大黄素的H-7(δH 6.56)、大黄素甲醚的H-7(δH 6.80)为定量目标信号,通过内标法测定大黄素、大黄素甲醚的含量。结果:本方法大黄素、大黄素甲醚的稳定性RSD分别为1.3%、0.8%;重复性RSD分别为3.2%、3.5%;日内精密度RSD分别为1.4%、0.3%;日间精密度RSD分别为0.9%、0.7%;大黄素、大黄素甲醚质量浓度分别在0.097~6.234、0.087~5.537 mg·mL-1范围内具有较好的线性关系,相关系数均为0.999;加样回收率均值分别为98.0%、99.2%,RSD分别为2.1%、2.4%。样品中大黄素、大黄素甲醚的含量分别为0.239~2.909、0.109~1.021 mg·g-1,与HPLC-UV所得数据基本一致。结论:所建立的氢核磁定量方法操作简单,测试时间短,且定量过程中不需要对照品,可用于何首乌及其炮制品的质量评价。
Objective: To propose an effective and simple quantitative 1H NMR method for the determination of emodin and physcion in raw and processed Polygoni Multiflori Radix.Methods: Diethyl sulfoxide-d6 was used as fest solution, δH6.25 was used as internal standard substance.The signals of H-7 of emodin (δH6.56)and physcion (δH6.80)were well separated for the quantitative analysis.The contents of emodin and physcion were determined by internal standard method.Results: The results showed that the RSD of stability, repeatability, intraday and interday precision for emodin were respectively 1.3%, 3.2%, 1.4% and 0.9%, and those for physcion were respectively 0.8%, 3.5%, 0.3% and 0.7%.Emodin and physcion showed good linearity in the ranges of 0.097-6.234 and 0.087-5.537 mg·mL-1 with correlation coefficients at 0.999, 0.999, respectively.The average percentage recoveries of emodin and physcion were respectively 98.0% and 99.2%, and the RSDs were 2.1%, 2.4%, respectively.The contents of emodin and physcion in tested samples were in the ranges of 0.239-2.909, 0.109-1.021 mg·g-1, respectively, and the results were found to be in reasonable agreement with those provided by HPLC-UV method.Conclusion: This method is rapid, reference-free and convenient with less sample pretreatment.