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LIU Huan; YU Xinmiao; WANG Yue; WANG Jiayue; LYU Xing; HOU Lijuan; LIN Ziwei; SUN Lixin

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更新时间：2023-03-01

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- China Pharmacy Vol. 30, Issue 14, (2019)
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LIU Huan, YU Xinmiao, WANG Yue, et al. [J]. China Pharmacy 30(14).(2019)
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LIU Huan, YU Xinmiao, WANG Yue, et al. [J]. China Pharmacy 30(14).(2019) DOI：

摘要

目的：建立胆木浸膏糖浆的高效液相色谱（HPLC）指纹图谱，并同时测定其中9种成分的含量。方法：采用HPLC法，色谱柱为Diamonsil C18（2），流动相为乙腈-0.1％磷酸溶液（梯度洗脱），流速为1.0 mL/min，检测波长为240 nm，柱温为30 ℃，进样量为10 μL。以异长春花苷内酰胺为参照，绘制20批胆木浸膏糖浆的HPLC图谱，采用《中药色谱指纹图谱相似度评价系统》（2004A版）进行相似度评价，确定共有峰，并通过标准曲线法测定9种成分的含量。结果：20批胆木浸膏糖浆的HPLC图谱有26个共有峰，相似度均大于0.98，通过与混合对照品比对，指认出9种化学成分，分别为原儿茶酸、新绿原酸、马钱苷酸、绿原酸、隐绿原酸、獐牙菜苷、短小蛇根草苷、异长春花苷内酰胺和喜果苷。这9种成分检测质量浓度的线性范围分别为17.24～275.84、7.56～120.96、15.40～246.40、7.84～125.44、8.64～138.24、7.96～127.36、8.40～134.40、48.56～776.96， 4.16～66.56 μg/mL（r均大于0.999）；检测限分别为0.043 1、0.126 0、0.038 5、0.130 7、0.144 0、0.066 3、0.070 0、0.012 1、0.052 0 μg/mL；定量限分别为0.215 5、0.189 0、0.077 0、0.196 0、0.288 0、0.132 7、0.105 0、0.097 6、0.138 7 μg/mL；精密度、稳定性、重复性试验的RSD均小于2.0％（n＝6），平均加样回收率分别为99.6％、106.3％、100.1％、102.0％、98.4％、100.0％、99.3％、100.6％、101.2％，RSD分别为1.20％、0.24％、0.59％、1.00％、0.73％、1.30％、1.10％、1.80％、1.90％（n＝6）。结论：所建立的胆木浸膏糖浆HPLC指纹图谱和定量测定方法分析准确度高、专属性强、灵敏度高，可以为胆木浸膏糖浆的质量控制提供参考。

Abstract

OBJECTIVE： To establish HPLC fingerprints of Nauclea officinalis extract syrup， and to determine the contents of 9 components. METHODS： HPLC method was adopted. The determination was performed on Diamonsil C18（2）column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid solution （gradient elution） at the flow rate of 1.0 mL/min. The detection wavelength was set at 240 nm， and column temperature was 30 ℃. The sample size was 10 μL. Using strictosamide as reference， HPLC chromatograms of 20 batches of N. officinalis extract syrup were drawn. The similarity of HPLC chromatograms were evaluated by using TCM Fingerprint Similarity Evaluation System （2004A edition） to confirm common peaks. The contents of 9 components were determined by standard curves. RESULTS： There were 26 common peaks in 20 batches of HPLC chromatograms， and the similarity was higher than 0.98. Compared with mixed control， 9 chemical components were identified， such as 3，4-dihydroxybenzoic acid， neochlorogenic acid， loganic acid， chlorogenic acid， cryptochlorogenic acid， swertioside， pumiloside， strictosamide and vincosamide. The linear range of 9 components were 17.24-275.84， 7.56-120.96， 15.40-246.40， 7.84-125.44， 8.64-138.24， 7.96-127.36， 8.40-134.40， 48.56-776.96， 4.16-66.56 μg/mL（all r≥0. 999）， respectively. The limits of detection were 0.043 1， 0.126 0， 0.038 5， 0.130 7， 0.144 0， 0.066 3， 0.070 0， 0.012 1， 0.052 0 μg/mL， respectively. The limits of quantitation were 0.215 5， 0.189 0， 0.077 0， 0.196 0， 0.288 0， 0.132 7， 0.105 0， 0.097 6， 0.138 7 μg/mL， respectively. RSDs of precision， stability and reproducibility tests were all lower than 2.0％（n＝6）. Average recoveries were 99.6％、106.3％、100.1％、102.0％、98.4％、100.0％、99.3％、100.6％ and 101.2％， and RSDs were 1.20％、0.24％、0.59％、1.00％、0.73％、1.30％、1.10％、1.80％、1.90％（n＝6）. CONCLUSIONS： Established HPLC fingerprints and quantitative determination method of N. officinalis extract syrup are accurate， specific and sensitive. It can provides reference for quality control of N. officinalis extract syrup.

关键词

胆木浸膏糖浆原儿茶酸新绿原酸马钱苷酸绿原酸隐绿原酸獐牙菜苷短小蛇根草苷异长春花苷内酰胺喜果苷高效液相色谱法指纹图谱含量测定

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