黄连黄柏提取液中3种生物碱的原位生成离子液体微萃取及HPLC测定

doi:10.3724/SP.J.1095.2013.30296

摘要/Abstract

摘要： 通过加入水溶性离子液体[C6MIM][Br]和离子对试剂NaPF6在黄连和黄柏的提取液中，原位生成非水溶性离子液体[C6MIM][PF6]萃取其生物碱，离心分相后，用HPLC测离子液体相中的生物碱小檗碱、巴马汀和黄连碱，其线性相关系数分别为0.9998、0.9996和0.9997，线性范围为1~2000 μg/L，检出限皆为0.5 μg/L，加标回收率96.52%~104.34%。这种方法可用于黄连和黄柏中的小檗碱、巴马汀和黄连碱的检测。

关键词: 生物碱, 离子液体, 原位溶剂生成微萃取, 高效液相色谱

Abstract: NaPF6 (as an ion-pairing agent) was added to the extraction solution of Rhizoma coptidis and Cortex phellodend containing [C6MIM][Br](as hydrophilic ionic liquid(IL)). A cloudy solution formed as a result of the formation of fine droplets of [C6MIM][PF6]. After centrifugation, the sedimented phase enriched with alkaloids was analyzed by HPLC with UV detection. In this method, several important parameters, such as the type and volume of ILs, the amount of NaPF6, solution pH, extraction time and centrifugation time, influencing the extraction efficiency of IL-ISFME(in situ solvent formation microextraction) were optimized. Under optimal conditions, berberine, palmatine and coptisine exhibit good linearity, with correlation coefficients of 0.9998, 0.9996 and 0.9997, respectively, a linear range of 1~2000 μg/L and the detection limit of 0.5 μg/L. The spiked recovery for each analyte is in the range of 96.52%~104.34%. The experimental results indicate that the proposed method is successfully applied to the analysis of three alkaloids in Rhizoma coptidis and Cortex phellodend.

Key words: alkaloids, ionic liquid, in situ solvent formation microextraction, high performance liquid chromatography

中图分类号:

O629. 3

曹玺珉, 吴昊, 张晋, 刘霞, 杜黎明. 黄连黄柏提取液中3种生物碱的原位生成离子液体微萃取及HPLC测定[J]. 应用化学, DOI: 10.3724/SP.J.1095.2013.30296.

CAO Ximin*, WU Hao, ZHANG Jin, LIU Xia, DU Liming. HPLC Determination of Three Alkaloids in Rhizoma coptidis and Cortex phellodend Microextracted with in situ Formed Ionic Liquids[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2013.30296.

参考文献

[1] Holbrey J D,Seddon K R. Ionic Iiquids[J]. Clean Products Processes,1999,1(4):223-236.

[2] Gutowski E K,Broker A G,Rogers D R,et al. Controlling the Aqueous Miscibility of Ionic Liquids:Aqueous Biphasic Systems of Water-miscible Ionic Liquids and Water-structuring Salt for Recycle, Metathesis and Separations[J] . J Am Chem Soc,2003,125:6632-6633.

[3] WANG Qiang,LIANG Hongze,BAO Weiliang. Preparation of Task-specific Ionic Liquids and Their Application in Organic Synthesis[J]. Chinese J Appl Chem,2007,24(2):117-122(in Chinese).

王强,梁洪泽,包伟良. 功能化离子液体的制备及其在合成中的应用[J]. 应用化学,2007,24(2):117-122.

[4] Huddleston J G,Willauer H D,Swatloski R P,et al. Temperature Ionic Liquids as Novel Media for ‘Clean’ Liquid-Liquid Extraction[J]. Chem Commun,1998,16:1765-1766.

[5] Poole C F,Poole S K. Extraction of Organic Compounds with Room Temperature Ionic Liquids[J]. J Chromatogr A,2010,1217:2268-2286.

[6] GUO Yanyan,YIN Weiping,LIU Pu,et al. Extraction and Separation of Isoflavonoids from Rhynchosia Volubilis Lour Using Ionic Liquid[J]. Chinese J Appl Chem,2011,28(5):537-541(in Chinese).

郭燕燕,尹卫平,刘普,等. 离子液体提取分离鹿藿中异黄酮化合物[J]. 应用化学,2011,28(5):537-541.

[7] Wu H,Du L M. Ionic Liquid-Liquid Phase Microextraction for the Sensitive Determination of Sanguinarine and Chelerythrine in Chinese Herbal Medicines and Human Urine[J]. J Liq Chromatogr R T,2012,35(12):1662-1675.

[8] Yao C,Anderson J L. Dispersive Liquid-Liquid Microextraction Using an in situ Metathesis Reaction to Form an Ionic Liquid Extraction Phase for the Preconcentration of Aromatic Compounds from Water[J]. Anal Bioanal Chem,2009,395:1491-1502.

[9] Mahpishanian S,Shemirani F. Preconcentration Procedure Using in situ Solvent Formation Microextraction in the Presence of Ionic Liquid for Cadmium Determination in Saline Samples by Flame Atomic Absorption Spectrometry[J]. Talanta,2010,82:471-476.

[10] Zeeb M,Ganjali M R,Norouzi P,et al. Separation and Preconcentration System Based on Microextraction with Ionic Liquid for Determination of Copper in Water and Food Samples by Stopped-flow Injection Spectrofluorimetry[J]. Food Chem Toxicol,2011,49:1086-1091.

[11] Mónica G H,Verónica P,Jared L A,et al. A Novel in situ Preconcentration Method with Ionic Liquid-based Surfactants Resulting in Enhanced Sensitivity for the Extraction of Polycyclic Aromatic Hydrocarbons from Toasted Cereals[J]. J Chromatogr A,2012,1227(3):29-37.

[12] Tsai Pilo,Tsai Tung hu. Simultaneous Determination of Berberine in Rat Blood, Liver and Bile Using Microdialysis Coupled to High-performance Liquid Chromatography[J]. J Chromatogr A,2002,961(1):125-130.

[13] Yin L H,Lu B N,Qi Y,et al. Simultaneous Determination of 11 Active Components in Two Well-known Traditional Chinese Medicines by HPLC Coupled with Diode Array Detection for Quality Control[J]. J Pharm Biomed Anal,2009,49(4):1101-1108.

[14] Deng Y T,Liao Q F,Li S H,et al. Simultaneous Determination of Berberine, Palmatine and Jatrorrhizine by Liquid Chromatography Tandem Mass Spectrometry in Rat Plasma and Its Application in a Pharmacokinetic Study after Oral Administration of Coptis Evodia Herb Couple[J]. J Chromatogr B,2008,863(2):195-205.

[15] Huang J M,Wang G Q,Jin Y,et al. Determination of Palmatine in Canine Plasma by Liquid Chromatography-tandem Mass Spectrometry with Solid-phase Extraction[J]. J Chromatogr B,2007,854:279-285.

[16] Yu S,Pang X Y,Deng Y X,et al. A sensitive and Specific Liquid Chromatography Mass Spectrometry Method for Simultaneous Determination of Berberine, Palmatine, Coptisine, Epiberberine and Jatrorrhizine from Coptidis Rhizoma in Rat Plasma[J]. Int J Mass Spectrom,2007,268:30-37.

[17] Chen J H,Wang F M,Liu J,et al. Analysis of Alkaloids in Coptis Chinensis Franch by Accelerated Solvent Extraction Combined with Ultra Performance Liquid Chromatographic Analysis with Photodiode Array and Tandem Mass Spectrometry Detections[J]. Anal Chim Acta,2008,613(2):184-195.

[18] Sun S W,Tseng H M. Sensitivity Improvement on Detection of Coptidis Alkaloids by Sweeping in Capillary Electrophoresis[J]. J Pharm Biomed Anal,2005,37(1):39-45.

编辑推荐 0

Metrics

阅读次数

全文

369

HTML			PDF

最新录用	在线预览	正式出版	最新录用	在线预览	正式出版
0	0	0	369	0	0

来源	本网站	其他网站

次数	366	3
比例	99%	1%

摘要

364

最新录用	在线预览	正式出版

364	0	0

	来源	本网站

	次数	364
	比例	100%