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采用高效液相色谱法同时测定延胡索(Pall.)中的 11 种异喹啉生物碱。

Simultaneous quantification of 11 isoquinoline alkaloids in Corydalis impatiens (Pall.) Fisch by HPLC.

机构信息

School of Medicine, Xi'an Jiaotong University, Xi'an City, PR China.

出版信息

J Sep Sci. 2013 Jul;36(13):2090-5. doi: 10.1002/jssc.201300036. Epub 2013 Jun 10.

Abstract

Isoquinoline alkaloids are the primary active ingredients of Corydalis, but an analytical method for quality assessment of the active ingredients in Corydalis impatiens (Pall). Fisch has not been reported. A new, simple, and multiple-component quantification method was developed for the simultaneous quantification of 11 isoquinoline alkaloids including capnoidine, chelianthifoline, bicuculline, protopine, isoapocavidine, apocavidine, cavidine, tetrahydroepiberberine, ochotensimine, tetrahydrocoptisine, and tetrahydrocorysamine in C. impatiens. Separation of the isoquinoline alkaloids was performed on a RP C18 column (150 × 4.6 mm, 5 μm) with potassium dihydrogen phosphate buffer (pH 2.5, adjusted by phosphoric acid)/acetonitrile (53:47, v/v) containing 0.3% sodium dodecyl sulfonate. The flow rate and detection wavelength were set at 1 mL/min and 295 nm, respectively. Full validation of the assay was carried out including linearity, precision, accuracy, stability, LOD, and limit of quantitation. All calibration curves showed a good linear relationship (r > 0.999) in test range. The results demonstrated that the developed method was reliable, rapid, and specific. Six batches of C. impatiens samples from different sources were determined using the established method. The contents of alkaloids ranged from 11.68 to 351.83 μg/g. This method can be applied for quality evaluation and control of C. impatiens. Eleven isoquinoline alkaloids were first reported on simultaneous determination with HPLC.

摘要

异喹啉生物碱是紫堇属的主要活性成分,但尚未报道用于评估延胡索(Pall)质量的分析方法。建立了一种新的、简单的、多组分定量方法,用于同时定量测定 11 种异喹啉生物碱,包括蝙蝠葛碱、刻叶紫堇灵、荷包牡丹碱、原阿片碱、异阿朴菲定、阿朴菲定、紫堇碱、延胡索乙素、紫堇诺林碱、四氢小檗碱和四氢刻叶紫堇碱。在 RP C18 柱(150×4.6mm,5μm)上分离异喹啉生物碱,采用磷酸氢二钾缓冲液(pH2.5,用磷酸调节)/乙腈(53:47,v/v),其中含有 0.3%十二烷基硫酸钠。流速和检测波长分别设定为 1mL/min 和 295nm。对该方法进行了全面验证,包括线性、精密度、准确度、稳定性、LOD 和定量限。在测试范围内,所有校准曲线均显示出良好的线性关系(r>0.999)。结果表明,所建立的方法可靠、快速且具有特异性。使用建立的方法测定了来自不同来源的 6 批延胡索样品。生物碱含量范围为 11.68 至 351.83μg/g。该方法可用于延胡索的质量评价和控制。首次采用 HPLC 同时测定了 11 种异喹啉生物碱。

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