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罂粟壳的HPLC指纹图谱建立及其5个成分的含量测定
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| 篇名： | 罂粟壳的HPLC指纹图谱建立及其5个成分的含量测定 |
| TITLE： | Establishment of HPLC Fingerprint and Content Determination of 5 Components in Papaveris Pericarpium |
| 摘要： | 目的：建立罂粟壳的指纹图谱，并测定其中吗啡、可待因、蒂巴因、罂粟碱、那可丁等5个成分的含量。方法：采用高效液相色谱（HPLC）法。以AgilentZORBAXEclipseXDB-C18为色谱柱，以甲醇-庚烷磺酸钠溶液为流动相进行梯度洗脱，流速为1.0mL/min，检测波长为238nm（罂粟碱）、216nm（吗啡、可待因、那可丁、蒂巴因），柱温为20℃，进样量为10µL。使用《中药色谱指纹图谱相似度评价系统（2012版）》建立15批罂粟壳药材样品的HPLC指纹图谱并进行相似度评价，结合混合对照品图谱确定共有峰；同法测定罂粟壳中吗啡、可待因、蒂巴因、罂粟碱、那可丁等5个成分的含量。采用SPSS19.0软件进行聚类分析。结果：15批罂粟壳药材样品中共有13个共有峰，相似度均大于0.99；共指认了5个色谱峰，分别为吗啡、可待因、蒂巴因、罂粟碱、那可丁。聚类分析结果显示，15批罂粟壳药材样品可聚为两类，S1～S7为聚为一类，S8～S15聚为一类，分属2个地市。吗啡等5个成分检测质量浓度的线性范围分别为10.21～102.10、10.43～104.30、1.54～30.70、2.36～47.28、2.32～57.90μg/mL（r均大于0.998）；精密度、稳定性（24h）、重复性试验的RSD均小于2％；平均加样回收率分别为99.46％（RSD＝1.08％，n＝6）、97.84％（RSD＝1.55％，n＝6）、91.10％（RSD＝1.74％，n＝6）、96.43％（RSD＝1.25％，n＝6）、94.82％（RSD＝1.20％，n＝6）；含量分别为2.3429～4.0822、0.4304～0.8897、0.0552～0.0904、0.2993～0.5588、0.3432～0.6562mg/g。结论：所建HPLC指纹图谱及含量测定方法简便可行、灵敏准确，结合聚类分析能较好地反映罂粟壳药材中化学成分的特征及内在质量；虽然不同地市产罂粟壳有区划特征，但质量基本稳定。 |
| ABSTRACT： | OBJECTIVE：To establish the fingerprint of Papaveris Pericarpium， and to determine the contents of 5 components，such as morphine ，codeine，thebaine，papaverine and narcotine. METHODS ：HPLC method was adopted. The determination was performed on a Agilent ZORBAX Eclipse XDB-C18 column with mobile phase consisted methanol -sodium heptanesulfonate with gradient elution at the flow rate of 1.0 mL/min. The detection wavelength were set at 238 nm（papaverine） and 216 nm（morphine，codeine，narcotine，thebaine）. The column temperature was 20 ℃，and sample size was 10 µL. HPLC fingerprints of 15 batches of Papaveris Pericarpium were established by using the Similarity Evaluation System of TCM Chromatographic Fingerprints （2012 edition），and the common peaks were determined in combination with the spectra of mixed control. The contents of morphine ，codeine，thebaine，papaverine and narcotine were determined simultaneously by the same method. The cluster analysis was conducted by using SPSS 19.0 software. RESULTS ：There were 13 common peaks in 15 batches of Papaveris Pericarpium ，and the similarity was greater than 0.99. Five chromatographic peaks were identified ，which were morphine，codeine，thebaine，papaverine and narcotin. The results of cluster analysis showed that 15 batches of Papaveris Pericarpium could be clustered into two categories ，S1-S7 and S 8-S15，belonging to two cities. The linear ranges of five components were 10.21-102.10，10.43-104.30，1.54-30.70，2.36-47.28，2.32-57.90 μg/mL，respectively（all r＞0.998）. RSDs of precision，stability（24 h）and repeatability tests were all less than 2％. The average recoveries were 99.46％（RSD＝1.08％，n＝ 6），97.84％（RSD＝1.55％，n＝6），91.10％（RSD＝1.74％，n＝6），96.43％（RSD＝1.25％，n＝6）、94.82％（RSD＝1.20％，n＝6）， respectively. The contents of 5 components were 2.342 9-4.082 2，0.430 4-0.889 7，0.055 2-0.090 4，0.299 3-0.558 8，0.343 2- 0.656 2 mg/g. CONCLUSIONS ：The established HPLC fingerprint and content determination method is simple ，feasible，sensitive and accurate. It combined with the cluster analysis could reflect characteristics and int ernal quality of chemical components in Papaveris Pericarpium . Papaveris Pericarpium in different cities possess regionalization characteristics ，but its quality isbasically stable. |
| 期刊： | 2021年第32卷第22期 |
| 作者： | 张晓萍，石晓峰，张虹艳，朱仁愿，张彩霞 |
| AUTHORS： | ZHANG Xiaoping ，SHI Xiaofeng ，ZHANG Hongyan ，ZHU Renyuan ，ZHANG Caixia |
| 关键字： | 罂粟壳；指纹图谱；聚类分析；含量测定；高效液相色谱法 |
| KEYWORDS： | Papaveris Pericarpium ；Fingerprint；Clustering |
| 阅读数： | 298 次 |
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