RP-HPLC 结合光电二极管阵列检测同时定量测定元胡止痛方中 12 种活性成分
Simultaneous Quantitative Determination of 12 Active Components in Yuanhu Zhitong Prescription by RP-HPLC Coupled with Photodiode Array Detection.
作者信息
Zhang Xiaokai, Zhang Song, Yang Qian, Cao Wei, Xie Yanhua, Qiu Pengcheng, Wang Siwang
机构信息
Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, Xi'an, China ; The Cultivation Project of Collaborative Innovation Center for Chinese Medicine in QinBa Mountains, Xi'an, China.
Pharmacy Department, Tangdu Hospital, Fourth Military Medical University, Xi'an, People's Republic of China.
出版信息
Pharmacogn Mag. 2015 Jan-Mar;11(41):61-8. doi: 10.4103/0973-1296.149705.
BACKGROUND
Yuanhu Zhitong prescription (YZP) is a famous traditional Chinese medicine formula, which is officially recorded in Chinese Pharmacopoeia for the treatment of stomach pain, hypochondriac pain, headache and dysmenorrhea caused by qi-stagnancy and blood stasis. It is the first report for the simultaneous determination of 12 active components in YZP.
OBJECTIVE
A newly, simple, accurate and reliable method for the separation and determination of 12 active components (protopine, α-allocryptopine, coptisine, xanthotol, palmatine, dehydrocorydaline, glaucine, tetrahydropalmatine, tetrahydroberberine, imperatorin, corydaline, isoimperatorin) in YZP was developed and validated using HPLC-PAD.
MATERIALS AND METHODS
The analytes were performed on a Phenomenex Luna-C18 (2) column (250×4.6 mm, 5.0 μm) with a gradient elution program using a mixture of acetonitrile and 0.1% phosphoric acid water solution (adjusted with triethylamine to pH 5.6) as mobile phase. Analytes were performed at 30°C with a flow rate of 1.0 mL/min.
RESULTS
The validated method was applied to analyze four major dosage forms of YZP coming from different manufacturers with good linearity (r(2), 0.99810.9999), precision (RSD, 0.242.89%), repeatability (RSD, 0.153.34%), stability (RSD, 0.143.35%), recovery (91.13~110.81%) of the 12 components.
CONCLUSION
The proposed method enables the separation and determination of 12 active components in a single run for the quality control of YZP.
背景
元胡止痛方是著名的中药方剂，已正式载入《中国药典》，用于治疗气滞血瘀所致的胃痛、胁痛、头痛及痛经。这是首次同时测定元胡止痛方中12种活性成分的报道。
目的
建立一种新的、简便、准确、可靠的方法，采用高效液相色谱-二极管阵列检测法（HPLC-PAD）分离并测定元胡止痛方中12种活性成分（原阿片碱、α-别隐品碱、黄连碱、黄藤素、巴马汀、去氢紫堇碱、青藤碱、延胡索乙素、四氢小檗碱、欧前胡素、紫堇碱、异欧前胡素），并进行方法学验证。
材料与方法
采用Phenomenex Luna-C18(2)色谱柱（250×4.6 mm，5.0μm），以乙腈和0.1%磷酸水溶液（用三乙胺调至pH 5.6）的混合溶液为流动相，采用梯度洗脱程序。柱温30℃，流速1.0 mL/min。
结果
该验证方法用于分析不同厂家生产的元胡止痛方的4种主要剂型，12种成分线性关系良好（r²，0.9981～0.9999），精密度（RSD，0.24～2.89%）、重复性（RSD，0.15～3.34%）、稳定性（RSD，0.14～3.35%）、回收率（%，91.13～110.81%）均良好。
结论
所建立的方法可一次进样分离并测定元胡止痛方中的12种活性成分，用于该制剂的质量控制。
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