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筋骨痛消丸HPLC指纹图谱的建立及其中7个成分的含量测定
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| 篇名： | 筋骨痛消丸HPLC指纹图谱的建立及其中7个成分的含量测定 |
| TITLE： | Establishment of HPLC Fingerprints and Content Determination of 7 Components of Jingu Tongxiao Pill |
| 摘要： | 目的：建立筋骨痛消丸的指纹图谱，并测定其中7个成分的含量。方法：采用高效液相色谱法（HPLC），以Cosmosil5C18-MS-Ⅱ为色谱柱，以乙腈-0.02％磷酸水溶液为流动相进行梯度洗脱，流速为1.0mL/min，检测波长为230nm，柱温为25℃，进样量为10μL。采用《中药色谱指纹图谱相似度评价系统（2012版）》建立10批筋骨痛消丸的HPLC指纹图谱并进行相似度评价，通过与混合对照品比对指认共有峰；采用同一HPLC法测定所指认共有峰对应成分的含量。结果：10批筋骨痛消丸样品中共确定共有峰20个，与对照指纹图谱的相似度均不低于0.980。通过与混合对照品比对，指认化学成分7个，分别为马钱苷酸、龙胆苦苷、芍药苷、丹酚酸B、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA。上述7个成分检测质量浓度的线性范围分别为4.509～45.090、15.090～150.900、14.985～149.850、14.982～149.820、2.967～29.670、1.944～19.440、3.094～30.940μg/mL（r均大于0.999），检测限分别为0.0601、0.1610、0.3996、0.1598、0.0316、0.0518、0.0825μg/mL，定量限分别为0.2004、0.5030、0.9990、0.3995、0.0791、0.2592、0.4126μg/mL；精密度、稳定性（24h）、重复性试验的RSD均小于3.0％（n＝6）；平均加样回收率为98.81％～100.28％，RSD为0.20％～1.21％（n＝6）。10批样品中上述成分的含量分别为0.4410～0.9694、3.2834～4.7334、1.9477～3.6749、1.3366～2.2709、0.2932～0.3721、0.1902～0.2939、0.3528～0.5188mg/g。结论：本研究成功建立了筋骨痛消丸的HPLC指纹图谱和含量测定方法，可用于其质量控制。 |
| ABSTRACT： | OBJECTIVE：To establish the fingerprint of Jingu tongxiao pill ，and to determine the contents of 7 components. METHODS：HPLC method was adopted. The determination was performed on Cosmosil 5C18-MS-Ⅱ column with acetonitrile- 0.02％ phosphoric acid solution as mobile phase （gradient elution ）at the flow rate of 1.0 mL/min. The detection wavelength was 230 nm and the column temperature was set at 25 ℃. The sample size was 10 μL. HPLC fingerprint of 10 batches of Jingu tongxiao pill was established by using Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition），and common peak was identified by comparing with the mixed reference substance. The contents of corresponding components of the identified common peak were determined by the same HPLC method. RESULTS ：There were 20 common peaks in HPLC fingerprint of 10 batches of samples ，and the similarity with the control fingerprint was not less than 0.980. By comparing with the mixed reference substance， 7 components were identified ， which were loganic acid ，gentiopicroside，paeoniflorin，salvianolic acid B ， cryptotanshinone，tanshinone Ⅰ and tanshinone Ⅱ A. The linear range of the above 7 components were 4.509-45.090， 15.090-150.900，14.985-149.850，14.982-149.820，2.967-29.670，1.944-19.440，3.094-30.940 μg/mL（all r＞0.999），respectively. The limits of detection were 0.060 1，0.161 0，0.399 6，0.159 8，0.031 6，0.051 8，0.082 5 μg/mL，respectively. The limits of quantitation were 0.200 4，0.503 0，0.999 0，0.399 5，0.079 1，0.259 2，0.412 6 μg/mL，respectively. RSDs of precision ，stability （24 h） and reproducibility tests were all lower than 3.0％ （n＝6）. Average recoveries were 98.81％ -100.28％ ，RSDs were 0.20％-1.21％（n＝6）. In 10 batches of samples ，the contents of the above 7 components were 0.441 0-0.969 4，3.283 4-4.733 4， 1.947 7-3.674 9，1.336 6-2.270 9，0.293 2-0.372 1，0.190 2-0.293 9 and 0.352 8-0.518 8 mg/g，respectively. CONCLUSIONS ：In this study，HPLC fingerprint and content determination method of Jingu tongxiao pill are successfully established and can be used for quality control. |
| 期刊： | 2021年第32卷第10期 |
| 作者： | 孙实，王一方，赵新杰，王昭，张丽，王丹丹，武爱玲，吴晓龙 |
| AUTHORS： | SUN Shi，WANG Yifang ，ZHAO Xinjie，WANG Zhao，ZHANG Li，WANG Dandan ，WU Ailing，WU Xiaolong |
| 关键字： | 筋骨痛消丸；指纹图谱；含量测定；高效液相色谱法 |
| KEYWORDS： | Jingu tongxiao pill ；Fingerprint；Content determination ；HPLC |
| 阅读数： | 254 次 |
| 本月下载数： | 6 次 |
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