Quantitative analysis of mephedrone using liquid chromatography tandem mass spectroscopy: Application to human hair

Shah, Syeda; Deshmukh, Nawed; Barker, James; Petróczi, Andrea; Cross, Paul; Archer, Roland; Naughton, Declan P.

doi:10.1016/j.jpba.2011.11.026

Cited by 40 publications

(34 citation statements)

References 13 publications

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“…Excellent peak shape and peak resolution were achieved for T, E and I.S. The accuracy, inter-day precision and intra-day precision of the assay were within the limits set by FDA guidelines [27] and are summarised in Supplementary Table S3. The extraction recovery results are summarised in Supplementary Table S4.…”

Section: Methods Validationmentioning

confidence: 62%

“…The performance of the analytical method was validated according to the FDA guidelines [27] for the following set of parameters: selectivity, accuracy, precision, lower limit of quantification (LLOQ), lower limit of detection (LLOD), linearity, extraction recoveries and sample stability. Samples for validation study were prepared by spiking 0.5 mg melanin with known concentrations of analytes and I.S.…”

Section: Methods Validationmentioning

confidence: 99%

“…Accuracy was evaluated by comparing the mean calculated values (6 replicates per concentration level) with the respective nominal concentration values [27]. Intra-day precision was determined by measuring 6 replicates per concentration level, on the same day.…”

Section: Methods Validationmentioning

confidence: 99%

“…LLOD was defined as the lowest concentration of the analyte which gave a peak response with a signal to noise ratio (S/N) of at least three. LLOQ was defined as the lowest concentration of the analyte: (i) which could be reliably quantified with a precision not exceeding 20% of the relative standard deviation and accuracy not deviating more than ±20% of the actual value, and (ii) which gave a peak response with a S/N of at least 10 [27]. Both LLOQ and LLOD were determined empirically using consecutive 1:2 dilutions of spiked samples.…”

Section: Methods Validationmentioning

confidence: 99%

See 3 more Smart Citations

Detection of testosterone and epitestosterone in human hair using liquid chromatography–tandem mass spectrometry

Deshmukh

Barker

Petróczi

et al. 2012

Journal of Pharmaceutical and Biomedical Analysis

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Section: Methods Validationmentioning

confidence: 62%

Section: Methods Validationmentioning

confidence: 99%

Section: Methods Validationmentioning

confidence: 99%

Section: Methods Validationmentioning

confidence: 99%

See 2 more Smart Citations

Detection of testosterone and epitestosterone in human hair using liquid chromatography–tandem mass spectrometry

Deshmukh

Barker

Petróczi

et al. 2012

Journal of Pharmaceutical and Biomedical Analysis

Self Cite

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“…In the analysis of drugs of abuse, blood and urine have become the most commonly used human sample matrices (33) , while only a few groups incorporate hair (34)(35)(36) or oral fluid. (37,38) Blood is often the matrix of choice because it is easy to obtain and because of its applicability to both ante-and post-mortem samples.…”

Section: Analysis Of Drugs Of Abuse In Biological Specimensmentioning

confidence: 99%

Comprehensive Forensic Toxicological Analysis of Designer Drugs

Swortwood¹

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When a positive result occurs, confirmatory methods, such as gas chromatography (GC) or liquid chromatography (LC) coupled with mass spectrometry (MS), are required for more sensitive and specific analyses. In recent years, the need to study the activities of these compounds in screening assays as well as to develop confirmatory techniques to detect them in biological specimens has been recognized. Severe intoxications and fatalities have been encountered with emerging designer drugs, presenting analytical challenges for detection and identification of such novel compounds. The first major task of this research was to evaluate the performance of commercially available immunoassays to determine if designer drugs were cross-reactive. The second major task was to develop and validate a confirmatory method, using LC-MS, to identify and quantify these designer drugs in biological specimens.vi Cross-reactivity towards the cathinone derivatives was found to be minimal.Several other phenethylamines demonstrated cross-reactivity at low concentrations, but results were consistent with those published by the assay manufacturer or as reported in the literature. Current immunoassay-based screening methods may not be ideal for presumptively identifying most designer drugs, including the "bath salts." For this reason, an LC-MS based confirmatory method was developed for 32 compounds, including eight cathinone derivatives, with limits of quantification in the range of 1-10 ng/mL. The method was fully validated for selectivity, matrix effects, stability, recovery, precision, and accuracy. In order to compare the screening and confirmatory techniques, several human specimens were analyzed to demonstrate the importance of using a specific analytical method, such as LC-MS, to detect designer drugs in serum as immunoassays lack cross-reactivity with the novel compounds. Overall, minimal crossreactivity was observed, highlighting the conclusion that these presumptive screens cannot detect many of the designer drugs and that a confirmatory technique, such as the LC-MS, is required for the comprehensive forensic toxicological analysis of designer drugs.vii

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Prevalence of new psychoactive substances: A retrospective study in hair

Rust

Baumgartner

Dally

et al. 2012

Drug Testing and Analysis

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New psychoactive substances are conquering the drug scene. Police seize different colourful packages with exceptional names. They are declared as 'bath salts', 'plant food', or 'research chemical powders'. Little is known about the actual prevalence of these drugs. Reanalysis of hair samples from routine cases concerning the presence of new psychoactive substances or 'smart drugs' should provide insight into changing patterns of designer drugs. All hair samples from 2009 and 2010 that originally tested positive for amphetamines or MDMA (N = 325) were reanalyzed for new or smart drugs such as 4-fluoroamphetamine, piperazines (BZP, mCPP and TFMPP), cathinones (4-MMC (mephedrone), methylone, butylone, ethylone, MDPV, methcathinone and cathinone), methylphenidate and ketamine. Hair snippets were extracted using a two-step extraction procedure. The analytes were analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) (electrospray ionization; multiple-reaction-monitoring mode - information dependent acquisition - enhanced product ion scan). New psychoactive substances were found in 120 cases (37%). Concerning the piperazine drugs, mCPP was positive in 34 (10.5%) cases and TFMPP in one case. Five mCPP cases were also positive for trazodone, an antidepressant which is metabolized to mCPP. In 11 (3%) cases, 4-MMC was detected. Concerning the smart drugs, methylphenidate was found in 16 (5%). Ketamine was found in 45 (14%) cases. 4-Fluoroamphetamine was identified in 12 (4%) cases and methylone in one case.In conclusion, there is a high prevalence of these drugs. Consequently, at least the most common ones (e.g. mCPP, KET, 4-MMC and 4-FA) should be included in screening procedures in clinical and forensic toxicology.

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Quantitative analysis of mephedrone using liquid chromatography tandem mass spectroscopy: Application to human hair

Cited by 40 publications

References 13 publications

Detection of testosterone and epitestosterone in human hair using liquid chromatography–tandem mass spectrometry

Detection of testosterone and epitestosterone in human hair using liquid chromatography–tandem mass spectrometry

Comprehensive Forensic Toxicological Analysis of Designer Drugs

Prevalence of new psychoactive substances: A retrospective study in hair

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