Ecstasy Analysis by Monolithic Materials-Capillary Electrochromatography

被引：7
作者：
Choodum, Aree [1 ,2 ]
Thavarungkul, Panote [3 ]
Kanatharana, Proespichaya [1 ,2 ]
Smith, Norman W. [4 ]
机构：
[1] Prince Songkla Univ, Dept Chem, Trace Anal & Biosensor Res Ctr, Hat Yai 90112, Songkhla, Thailand
[2] Prince Songkla Univ, Ctr Excellence Innovat Chem, Fac Sci, Hat Yai 90112, Songkhla, Thailand
[3] Prince Songkla Univ, Fac Sci, Dept Phys, Trace Anal & Biosensor Res Ctr, Hat Yai 90112, Songkhla, Thailand
[4] Kings Coll London, Pharmaceut Sci Res Div, Micro Separat Grp, London SE1 9NH, England
来源：
ANALYTICAL SCIENCES | 2009年 / 25卷 / 04期
关键词：
PERFORMANCE LIQUID-CHROMATOGRAPHY; REVERSED-PHASE; 3,4-METHYLENEDIOXYMETHAMPHETAMINE MDMA; STEREOCHEMICAL ANALYSIS; STATIONARY PHASES; MAIN METABOLITES; URINE; AMPHETAMINE; PLASMA; SEPARATION;
D O I：
10.2116/analsci.25.517
中图分类号：
O65 [分析化学];
学科分类号：
070302 ; 081704 ;
摘要：
Monolithic columns were successfully prepared and used with capillary electrochromatography for the analysis of 3,4-methylenedioxymethamphetamine (MDMA) in ecstasy tablets and its metabolites in urine samples. Cationic and neutral monolith columns provided better efficiencies than anionic monoliths. The neutral butyl methacrylate (BMA) monolith column provided symmetrical peaks with the highest efficiency, high resolution and short analysis times. The developed method using BMA monolithic column provided the detection limits for MDMA and its metabolites at 1 mu g mL(-1) with excellent intra-day and inter-day precision and linearity from 7.5 to 100 mu g mL(-1) (R-2 >= 0.99). MDMA was found as the main component in ecstasy tablets while 4-hydroxy-3-methoxymethamphetamine as the major metabolite in urine samples. High recoveries (97% for MDMA from tablets and 84 - 102% for its metabolites from urine samples) were obtained using simple ultrasonic extraction for ecstasy tablets and liquid-liquid extraction for urine samples.
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收藏
页码：517 / 522
页数：6
相关论文
共 51 条
[1]   Sintered octadecylsilica as monolithic column packing in capillary electrochromatography and micro high-performance liquid chromatography [J].
Asiaie, R ;
Huang, X ;
Farnan, D ;
Horváth, C .
JOURNAL OF CHROMATOGRAPHY A, 1998, 806 (02) :251-263
[2]   Theory of capillary electrochromatograpy [J].
Bartle, KD ;
Myers, P .
JOURNAL OF CHROMATOGRAPHY A, 2001, 916 (1-2) :3-23
[3]   Capillary electrochromatography with monolithic stationary phases - II. Preparation of cationic stearyl-acrylate monoliths and their electrochromatographic characterization [J].
Bedair, M ;
El Rassi, Z .
JOURNAL OF CHROMATOGRAPHY A, 2003, 1013 (1-2) :35-45
[4]  
CLIMKO RP, 1986, INT J PSYCHIAT MED, V16, P359
[5]   The content of ecstasy tablets: implications for the study of their long-term effects [J].
Cole, JC ;
Bailey, M ;
Sumnall, HR ;
Wagstaff, GF ;
King, LA .
ADDICTION, 2002, 97 (12) :1531-1536
[6]  
deBoer D, 1997, J MASS SPECTROM, V32, P1236
[7]   Capillary electrochromatography - A high-efficiency micro-separation technique [J].
Dittmann, MM ;
Rozing, GP .
JOURNAL OF CHROMATOGRAPHY A, 1996, 744 (1-2) :63-74
[8]   Separation of basic solutes by reversed-phase capillary electrochromatography [J].
Dittmann, MM ;
Masuch, K ;
Rozing, GP .
JOURNAL OF CHROMATOGRAPHY A, 2000, 887 (1-2) :209-221
[9]   Capillary electrochromatography with a neutral monolithic column for classification of analytes and determination of basic drugs in human serum [J].
Dong, J ;
Xie, CH ;
Tian, RJ ;
Wu, RN ;
Hu, JW ;
Zou, HF .
ELECTROPHORESIS, 2005, 26 (18) :3452-3459
[10]   The use of cyclohexanone as a "derivatizing" reagent for the GC-MS detection of amphetamines and ephedrines in seizures and the urine [J].
El-Haj, BM ;
Al-Amri, AM ;
Hassan, MH ;
Ali, HS ;
Bin Khadem, RK .
FORENSIC SCIENCE INTERNATIONAL, 2003, 135 (01) :16-26
123456