Luo Ding-Qiang, Jia Pu, Zhao Shan-Shan, Zhao Ye, Liu Hai-Jing, Wei Feng, Ma Shuang-Cheng
Shaanxi Institute for Food and Drug Control, Xi'an 710065, China.
Northwest University, Xi'an 710069, China.
J Anal Methods Chem. 2019 Aug 8;2019:7430717. doi: 10.1155/2019/7430717. eCollection 2019.
The quantitative analysis of multicomponents by the single-marker (QAMS) method was established and the relationship between value (the ratio of the sum of the contents of emodin-8-O--D-glucopyranoside and physcion-8-O--D-glucopyranoside to the sum of the contents of emodin and physcion) and the steaming time was found to identify and differentiate Radix and its processed product. Emodin was considered as the control substance, and the correction factors of physcion, emodin-8-O--D-glucopyranoside, and physcion-8-O--D-glucopyranoside were computed. In addition, the contents of the four components were determined. When the value is greater than or equal to 1.0, the sample was identified as Radix, and if the value was between 0.6 and 1.0, the sample of Radix Preaparata was processed incompletely. The value of the qualified Radix should be no more than 0.6. However, the influence of different sample injection volumes and the chromatographic columns and instruments used on the durability of the correction factors and RSD ≤3% hindered accurate identification; therefore, a QAMS method using an external standard value with methodological verification was developed. We redefined the " rules." The method using " rules" revised after optimization of the determination results was used, as it was accurate and led to convenient operation and low inspection costs, and moreover, the method could differentiate Radix Preaparata and Radix medicinal samples and precisely identify samples that were different from the completely processed product Radix Preaparata.
建立了单指标多成分定量分析（QAMS）方法，通过测定值（大黄素-8-O-β-D-吡喃葡萄糖苷与大黄酚-8-O-β-D-吡喃葡萄糖苷含量之和与大黄素和大黄酚含量之和的比值）与蒸制时间的关系来鉴别和区分大黄及其炮制品。以大黄素为对照品，计算大黄酚、大黄素-8-O-β-D-吡喃葡萄糖苷、大黄酚-8-O-β-D-吡喃葡萄糖苷的校正因子。此外，测定了4种成分的含量。当测定值大于或等于1.0时，样品鉴定为大黄；当测定值在0.6至1.0之间时，大黄炮制品加工不完全。合格大黄的测定值应不超过0.6。然而，不同进样量以及所使用的色谱柱和仪器对校正因子耐用性的影响以及RSD≤3%阻碍了准确鉴别；因此，开发了一种采用外标值并进行方法学验证的QAMS方法。我们重新定义了“规则”。采用优化测定结果后修订的“规则”方法，因为该方法准确，操作简便，检测成本低，而且该方法能够区分大黄炮制品和大黄药材样品，并能精确鉴别与完全炮制的大黄炮制品不同的样品。
