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基于超高效液相色谱技术的不同加工时间女贞子炮制品主要成分含量变化及其特征性质量标准研究

[Content change of main components in processed Ligustrum lucidum fruits of different processing time and their characteristic quality standard based on UPLC technology].

作者信息

Ji Xin, Liu Xiao-Qian, Li Chun, Yang Li-Xin, Feng Wei-Hong, Wang Zhi-Min

机构信息

National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines, Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2018 Dec;43(24):4862-4868. doi: 10.19540/j.cnki.cjcmm.20181105.012.

Abstract

To investigate the dynamic change law of the main components in Ligustri Lucidi Fructus during the wine-steaming process and attempt to establish the characteristic quality standard of wine-steamed Ligustri Lucidi Fructus by determining the content of salidroside and specnuezhenide using Ultra Performance Liquid Chromatography (UPLC) technology at different processing time points (12, 15, 18, 21, 24 h). The chromatographic separation was performed on Waters Acquity UPLC®BEH C₁₈ column (2.1 mm×50 mm, 1.7 μm) with acetonitrile and 0.2% formic acid aqueous solution as the mobile phase for gradient elution; and the detection wavelength was set at 280 nm; the flow rate was 0.5 mL·min⁻¹, and the column temperature was set at 40 °C. The results showed that the two components were well separated in the above conditions. The salidroside and specnuezhenide showed a good linear relationship within the range of 10.19-326 ng and 49.53-1 585 ng, respectively. Their average recovery was 103.4% and 101.7% with RSD of 0.81% and 0.79%, respectively. With the extension of processing time, the content of specnuezhenide was decreased, while salidroside was gradually increased. For the 27 batches of Ligustri Lucidi Fructus, the content of salidroside was between 0.042 5% and 0.192 4%, and that of specnuezhenide was between 0.829 7% and 5.218 0%. While for the 25 batches of wine-steamed Ligustri Lucidi Fructus, the content of the first one was between 0.229 2% and 1.045 8%, and the latter one was between 0.743 8% and 3.645 4%. As compared with Ligustri Lucidi Fructus, the ratio of specnuezhenide to salidroside was significantly decreased in the wine-steamed Ligustri Lucidi Fructus. According to the experimental results, the quality standard of Ligustri Lucidi Fructus is tentatively fixed as follows: the content of specnuezhenide shall not be less than 0.80%, and the ratio of specnuezhenide content/salidroside content (Sp/Sa) should not be smaller than 15. As for the wine-steamed ones, the content of salidroside should not be less than 0.20%, and specnuezhenide content should not be less than 0.70%; Sp/Sa should not be greater than 8. The method established in this study is simple and reliable, which could be used for the content detection of salidroside and specnuezhenide in Ligustri Lucidi Fructus samples. The characteristic quality standard established in this study could be used to distinguish the Ligustri Lucidi Fructus and wine-steamed Ligustri Lucidi Fructus.

摘要

为研究女贞子酒蒸过程中主要成分的动态变化规律,并尝试通过超高效液相色谱(UPLC)技术测定不同加工时间点(12、15、18、21、24 h)的红景天苷和特女贞苷含量,建立酒蒸女贞子的特征质量标准。采用Waters Acquity UPLC®BEH C₁₈色谱柱(2.1 mm×50 mm,1.7 μm)进行色谱分离,以乙腈和0.2%甲酸水溶液为流动相进行梯度洗脱;检测波长设定为280 nm;流速为0.5 mL·min⁻¹,柱温设定为40℃。结果表明,上述条件下两种成分分离良好。红景天苷和特女贞苷分别在10.19 - 326 ng和49.53 - 1585 ng范围内呈良好的线性关系。它们的平均回收率分别为103.4%和101.7%,相对标准偏差分别为0.81%和0.79%。随着加工时间的延长,特女贞苷含量降低,而红景天苷逐渐增加。27批女贞子中,红景天苷含量在0.0425%至0.1924%之间,特女贞苷含量在0.8297%至5.2180%之间。而25批酒蒸女贞子中,前者含量在0.2292%至1.0458%之间,后者含量在0.7438%至3.6454%之间。与女贞子相比,酒蒸女贞子中特女贞苷与红景天苷的比值显著降低。根据实验结果,女贞子的质量标准暂定为:特女贞苷含量不得低于0.80%,特女贞苷含量/红景天苷含量(Sp/Sa)比值不得小于15。对于酒蒸女贞子,红景天苷含量不得低于0.20%,特女贞苷含量不得低于0.70%;Sp/Sa不得大于8。本研究建立的方法简便可靠,可用于女贞子样品中红景天苷和特女贞苷的含量检测。本研究建立的特征质量标准可用于区分女贞子和酒蒸女贞子。

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