Simultaneous gas chromatographic determination of methamphetamine, amphetamine and their p-hydroxylated metabolites in plasma and urine

Cheung, Siu Wah; Nolte, Hans-Jürgen; Otton, S V; Tyndale, Rachel F.; Wu, Pin; Sellers, Edward M.

doi:10.1016/s0378-4347(96)00361-1

Cited by 38 publications

(21 citation statements)

References 17 publications

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“…In hair samples, AP and MP could also be detected in very low concentrations. al., , Jonsson et al, 1996Herraez-Hernandez et al, 1998), in addition to plasma (Cheung et al, 1997;Nakashima et al, 1990;Nagasawa et al, 1996;Gjerde et al, 1993;Hara et al, 1997;Bogusz et al, 1997) and hair (Nakahara et al, 1993;Slawson et al, 1996;Takayama et al, 1997), have been detailed.Recently, we reported highly sensitive HPLC methods with fluorescence (FL) detection for the determination of AP and MP in urine (Al-Dirbashi et al, 1998a,b, 2000a and hair samples (Al-Dirbashi et al, 1999, 2000b obtained from MP abusers. In these methods, AP and MP were determined after their derivatization with the fluorescent reagent, 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride (DIB-Cl) (Nakashima et al, 1995).…”

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confidence: 99%

Determination of methamphetamine and amphetamine in abusers' plasma and hair samples with HPLC‐FL

Nakashima

Kaddoumi

Ishida

et al. 2003

Biomedical Chromatography

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This paper describes highly sensitive HPLC methods for the determination of amphetamine (AP) and methamphetamine (MP) in abusers' plasma and hair samples. AP and MP were derivatized with the fluorescent reagent, DIB-Cl, to yield a highly fluorescent DIB-derivatives of AP and MP, which were then analyzed by HPLC with fluorescence detection at excitation and emission wavelengths of 325 and 430 nm, respectively. The separation was achieved on an ODS column with isocratic mobile phases composed of acetoniltrile and citrate buffer (55:45, v/v) for plasma samples and of acetonitrile-methanol-citrate buffer (45:20:37.5, v/v/v) for hair samples. The limits of detection were less than 0.87 ng/mL and 0.12 ng/mg in plasma and hair samples, respectively, for both AP and MP. The methods were then applied to the determination of MP and its metabolite AP in plasma obtained from two cases of illegally ingested MP and in one of the cases' hair received later. Case I was treated with dialysis; samples before and after dialysis were analyzed by the described method. After dialysis for 5 h, the total plasma levels of AP and MP decreased from 720 to 190 ng/mL. For case II, MP and AP levels were monitored for 3 days after digestion. Total plasma levels decreased from 57 ng/mL in the day of digestion to 11 ng/mL after 3 days. In hair samples, AP and MP could also be detected in very low concentrations.

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confidence: 99%

Determination of methamphetamine and amphetamine in abusers' plasma and hair samples with HPLC‐FL

Nakashima

Kaddoumi

Ishida

et al. 2003

Biomedical Chromatography

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“…The detection limits calculated were in a range from 4 to 97 fmol/injection at a signal-tonoise ratio (S/N) of 3. This sensitivity is almost comparable to that for an HPLC-UV method employing sodium naphthoquinone-4-sulphonate as a derivatizing reagent 13) and a GC method with a nitrogen-phosphorus detector, 3) but lower than that of GC-MS 7,8) and HPLC-FL methods.…”

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confidence: 82%

“…For the analysis of some of these drugs, gas chromatography (GC), [2][3][4] GC-mass spectrometry (GC-MS) [5][6][7][8][9] and high-performance liquid chromatography (HPLC) [10][11][12][13][14] are exclusively employed. GC-MS methods are generally highly sensitive but require a derivatization procedure prior to the analysis.…”

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confidence: 99%

Separation of Sympathomimetic Amines of Abuse and Related Compounds by Micellar Electrokinetic Chromatography.

Kuroda

Sato

Ohyama

et al. 2001

CHEMICAL & PHARMACEUTICAL BULLETIN

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Methamphetamine (MP) and amphetamine (AP) are wellknown drugs of abuse and the illicit use of MP is spreading and causing serious social problems in Japan. The use of these stimulants is controlled by the Stimulants Control Law for drug offenses. 4-Bromo-2,5-dimethoxyphenylethylamine (2C-B) which has an intensely hallucinogenic effect was also designated as a "narcotic" and has been controlled by the Narcotics and Psychotropic Control Law since 1998. In addition to these drugs, anorectic drugs such as phentermine (PT) and fenfluramine (FF) were illegally used as adulterants in commercial Chinese tea a few years ago in Japan.1) Due to the increasing diversity of drugs of abuse, a rapid and simple analysis which can be applied to a wide range of analytes for qualitative and quantitative purposes is required in forensic and toxicological studies.For the analysis of some of these drugs, gas chromatography (GC), 2-4) GC-mass spectrometry (GC-MS) 5-9) and high-performance liquid chromatography (HPLC) [10][11][12][13][14] are exclusively employed. GC-MS methods are generally highly sensitive but require a derivatization procedure prior to the analysis.5-9) HPLC methods with fluorescence (FL), 11,14) chemiluminescence (CL) 12) and UV-Vis 10,13) detections also require derivatization to increase the sensitivity and a rather long time to separate analytes. As an analytical technique to meet the requirements for the applicability to diverse analytes, capillary electrophoresis (CE) has been developed. 15) We previously described the usefulness of CE with UV absorbance detection for simultaneous determination of six kinds of stimulants and related compounds in urine samples. 16) In this study, we have expanded the analytes to include other amines [i.e., l-deprenyl (DPN, a prescription drug for Parkinsonism that is metabolized to R(Ϫ)-AP and R(Ϫ)-MP), methylephedrine (ME, a starting material of stimulants), 2C-B (a narcotic) and PT, FF and Mazindol (MZ) (anorexics)], and investigated their separation and detection using micellar electrokinetic chromatography (MEKC). Since the present method is expected to be effective as a rapid and simple qualitative and quantitative analysis for seized drugs and their adulterated foods, its applicability was investigated by applying it to the determination of PT spiked into Chinese tea leaves. ExperimentalChemicals and Materials 1-Phenylethylamine (1-PA), 2-phenylethylamine (2-PA), PT and FF were purchased from Sigma-Aldrich Japan (Tokyo). MP hydrochloride was obtained from Dainippon Pharmacy (Osaka, Japan). AP sulfate, 4-hydroxyamphetamine (4-HAP), and 4-hydroxymethamphetamine (4-HMP) were synthesized in our laboratory and 2C-B was synthesized by one of the authors. ME and MZ were the gifts of Dainippon Pharmacy and Sandoz Pharmaceutical, Ltd. (Tokyo, Japan), respectively. DPN was supplied by Fujimoto Pharmaceutical Co. (Osaka, Japan). These compounds were dissolved in water to give 0.01 M solutions and then diluted with water to appropriate concentrations prior to use. Sodium tetraborate ...

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“…[4][5][6][7][8] In the present paper, we describe the development and optimization of the method for the direct determination of intact p-OHMA glucuronide (p-OHMAG). Even in a case where the concentration of AP present in the urine is too low to be determined, it has been reported that the levels of p-OHMA and its conjugated form excreted in the urine were much higher than AP.…”

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confidence: 99%

“…3) It has been reported in the literature that the analysis of conjugated forms of p-OHMA in the urine samples of MA abusers used to be carried out by comparing the ratios of free p-OHMA to total p-OHMA before and after hydrolysis with b-glucuronidase or HCl treatment. [4][5][6][7][8] In the present paper, we describe the development and optimization of the method for the direct determination of intact p-OHMA glucuronide (p-OHMAG). Even in a case where the concentration of AP present in the urine is too low to be determined, it has been reported that the levels of p-OHMA and its conjugated form excreted in the urine were much higher than AP.…”

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Direct Determination of p-Hydroxymethamphetamine Glucuronide in Human Urine by High-Performance Liquid Chromatography

Nakajima

Morishita

Aiso

et al. 2006

CHEMICAL & PHARMACEUTICAL BULLETIN

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Drug abuse has recently become a serious worldwide problem and is increasing rapidly. Illicit drugs are stimulants, marijuana, cocaine, heroin and tranquilizers, among which methamphetamine (MA) is the most frequently abused drug in Japan. Arrests for violation of the Stimulant Drug Control Law are now on the verge of 20000/year. MA addiction is evidenced by the detection of unchanged MA as well as metabolite amphetamine (AP), thus MA analysis in urine samples has been employed routinely as a standard screening test using thin layer chromatography (TLC), 1) followed by gas chromatography/mass spectrometry (GC/MS).2) MA is metabolized either by hydroxylation of the aromatic ring or demethylation of the side chain. It has been reported that the metabolites of MA in urine were excreted as the unchanged (18-27%), free and conjugated forms of p-hydroxymethamphetamine (p-OHMA; 14-16%) and AP (2-3%) (Fig. 1). 3)It has been reported in the literature that the analysis of conjugated forms of p-OHMA in the urine samples of MA abusers used to be carried out by comparing the ratios of free p-OHMA to total p-OHMA before and after hydrolysis with b-glucuronidase or HCl treatment. [4][5][6][7][8] In the present paper, we describe the development and optimization of the method for the direct determination of intact p-OHMA glucuronide (p-OHMAG). Even in a case where the concentration of AP present in the urine is too low to be determined, it has been reported that the levels of p-OHMA and its conjugated form excreted in the urine were much higher than AP. We are thus convinced that a simultaneous determination of p-OHMAG, p-OHMA and MA in the urine of MA abusers could be unambiguous evidence of the ingestion of MA. ExperimentalMaterials and Reagents p-Hydroxymethamphetamine glucuronide (p-OHMAG) was synthesized from 4-hydroxyphenylacetic acid methyl ester according to the method developed in our laboratory.9) Pholedrine, p-hydroxymethamphetamine (p-OHMA) and methamphetamine (MA) hydrochloride were obtained from Sigma (St. Louis, MO, U.S.A.) and Dainippon Pharmaceutical (Osaka, Japan), respectively (Fig. 1). Sodium 1-dodecanesulfonate (ion pair grade) was purchased from Tokyo Kasei Kogyo (Tokyo, Japan). Methanol and acetonitrile were of HPLC grade, and all other reagents were of analytical grade.Standard solutions: the concentrations of a standard solution were set in the vicinity of the limits of quantification (LOQ). Stock solutions were prepared by dissolving appropriate amounts of p-OHMAG, p-OHMA and MA in distilled water and were kept frozen until use, then diluted appropriately prior to use.Distilled and deionized water prepared with Elix (Millipore, Tokyo) was used throughout this investigation.Sep-Pak ® Light C18 cartridges (reversed-phase monofunctional silane, 130 mg) were obtained from Waters Corp. (Milford, MA, U.S.A.).A drug free urine sample collected from a healthy subject in our laboratory was used to make blank and spiked urine samples containing standard solutions. The urine samples of MA abusers were obtained f...

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Simultaneous gas chromatographic determination of methamphetamine, amphetamine and their p-hydroxylated metabolites in plasma and urine

Cited by 38 publications

References 17 publications

Determination of methamphetamine and amphetamine in abusers' plasma and hair samples with HPLC‐FL

Determination of methamphetamine and amphetamine in abusers' plasma and hair samples with HPLC‐FL

Separation of Sympathomimetic Amines of Abuse and Related Compounds by Micellar Electrokinetic Chromatography.

Direct Determination of p-Hydroxymethamphetamine Glucuronide in Human Urine by High-Performance Liquid Chromatography

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