Matrix effect in bio-analysis of illicit drugs with LC-MS/MS: Influence of ionization type, sample preparation, and biofluid

Dams, R.; Huestis, Marilyn A.; Lambert, Willy E.; Murphy, Constance M.

doi:10.1016/s1044-0305(03)00574-9

Cited by 554 publications

(390 citation statements)

References 15 publications

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“…In addition, the complex mixture of compounds in the urine matrix did not significantly interfere in the direct detection of the selected ATS. On the other hand, severe matrix effects emerge during the LC-MS/MS analysis of drugs, mainly because the electrospray source (ESI-MS) is highly susceptible to other components present in the matrix, which may result in signal suppression or enhancement [13].…”

Section: Resultsmentioning

confidence: 99%

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Crevelin

Salami

Alves

et al. 2016

J. Am. Soc. Mass Spectrom.

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Time Intensity Q1Q2 CID ASAP Probe Corona ConeAbstract. Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

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Section: Resultsmentioning

confidence: 99%

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Crevelin

Salami

Alves

et al. 2016

J. Am. Soc. Mass Spectrom.

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“…Co-elution of molecules or elution of isobaric molecules in the matrix is often an issue when analysing urine samples using HPLC-MS [31]. Although simple dilution of urine samples is suggested to be enough for making urine samples compatible for LC-MS analysis [32]. However simple dilution is not recommended for metabolomic studies because this procedure does not remove unwanted larger molecules.…”

Section: Matrix Effectmentioning

confidence: 99%

Development of Zwitterionic Hydrophilic Liquid Chromatography (ZICⓇHILIC-MS) Metabolomics Method for Shotgun Analysis of Human Urine

Trivedi¹,

Jones²,

Shah³

et al. 2012

J Chromatogr Sep Tech

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“…The efficiency of DVS and IS extraction from rabbit plasma was determined by comparing the responses of the analytes extracted from replicate QC samples (n = 6) with the response of analytes from post extracted plasma standard sample at equivalent concentrations by liquid-liquid extraction [15]. Recoveries of DVS were determined at QC low and QC high concentrations, i.e.…”

Section: Recoverymentioning

confidence: 99%

A Highly Sensitive LC-Ms/Ms Method for Determination of Desvenlafaxine in Rabbit Plasma and its Application to Rabbit Pharmacokinetic Study

Reddy¹

2011

J Anal Bioanal Tech

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A highly senstive and rapid LC-MS/MS method has been developed and validated for the estimation of desvenlafaxine in rabbit plasma. The chromatographic separation was performed with 0.2% formic acid: methanol at flow rate of 0.4 mL/min on Symmetry Shield RP18 column with a total run time of 3.0 min. TheMS/MS ion transitions monitored were 263.90 58.10 for desvenlafaxine and 281.30 86.10 for IS (metaprolol). Method validation and pre-clinical sample analysis were performed as per FDA guide lines and the results met the acceptance crieteria. The lower limit of quantification achieved was 0.5 ng/mL and the linearity was observed from 0.5 to 1500ng/mL. This novel method has been applied to pharmacokinetic study of desvenlafaxine in rabbits. Page 2 of 6 10ASvp) and auto-sampler (SIL-HTC) along with a system controller (SCL-10Avp) was used to inject 2 μL aliquots of the processed samples on a Symmetry Shield RP18 column (50 x 4.6 mm, 3.5 μm, Waters Corporation, Ireland, UK), which was kept at ambient temperature (24 ± 2°C). The isocratic mobile phase, a mixture of 0.2% formic acid and methanol mixture (20:80, v/v) was filtered through a 0.45 μm membrane filter (Millipore) and then degassed ultrasonically for 5 min was delivered at a flow rate of 0.40 mL/min into the mass spectrometer electro spray ionization chamber. Mass spectrometry operating conditionsQuantification was achieved by MS/MS detection in positive ion mode for analyte and IS using a MDS Sciex (Foster City, CA, USA) API 4000 mass spectrometer, equipped with a Turboionspray™ interface at 500°C. The common parameters, i.e. curtain gas, nebulizer gas, auxillary gas and collision gas, were set at 10, 35, 40 and 6 psi, respectively. The compounds parameters, i.e. declustering potential (DP), collision energy (CE), collision exit potential (CXP) and entrance potential (EP) for DVS and IS were 60, 43, 8, 10 V and 44, 26, 8, 10 V, respectively. Detection of the ions was performed in the multiple reaction monitoring (MRM) mode, monitoring the transition of the m/z 263.90 precursor ion to the m/z 58.10 product ion for DVS and m/z 281.30 precursor ion to the m/z 86.10 product ion for IS. Quadrupole Q1 was set on low resolution where as Q3 was set on unit resolution. The analytical data were processed by Analyst software (version 1.4.2). Preparation of stock and standard solutionsPrimary stock solutions of DVS for preparation of standard and quality control (QC) samples were prepared from separate weighing. The primary stock solutions were prepared in methanol (1000 μg/mL). The IS stock solution of 1000 μg/mL was prepared in methanol. The stock solutions of DVS and IS were stored at 4°C, which were found to be stable for one month (data not shown) and successively diluted with methanol to prepare working solutions to prepare the calibration curve (CC). Another set of working stock solutions of DVS were made in methanol (from primary stock) for preparation of QC samples. Working stock solutions were stored at approximately 4°C for a week (data not shown). A...

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Matrix effect in bio-analysis of illicit drugs with LC-MS/MS: Influence of ionization type, sample preparation, and biofluid

Cited by 554 publications

References 15 publications

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Development of Zwitterionic Hydrophilic Liquid Chromatography (ZICⓇHILIC-MS) Metabolomics Method for Shotgun Analysis of Human Urine

A Highly Sensitive LC-Ms/Ms Method for Determination of Desvenlafaxine in Rabbit Plasma and its Application to Rabbit Pharmacokinetic Study

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