Determination of LSD and its metabolites in human biological fluids by high-performance liquid chromatography with electrospray tandem mass spectrometry

Canezin, J; Cailleux, A.; Turcant, Alain; Bouil, Anne Le; Harry, P.; Allain, Pierre

doi:10.1016/s0378-4347(01)00386-3

Cited by 56 publications

(52 citation statements)

References 20 publications

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“…at m/z 309 and [MH-C 2 H 5 ] +. at m/z 293 but neither were observed in ESI and CID conditions in a triple quadrupole [6,10]. To detect further fragmentation pathways, MS 3 experiments were also performed on CID-generated ion species at m/z 281 and 223 (see Table 1) at tickle voltage of 28 and 35%, respectively.…”

Section: Ms/msmentioning

confidence: 99%

“…Of the various analytical approaches which have been proposed in the last decade, a leading role has been played by those employing multiple mass spectrometry (MS/MS) features which allow the mise au point of specific and sensitive methods based either on gas chromatographymultiple mass spectrometry (GC-MS/MS) or liquid chromatography-multiple mass spectrometry (LC-MS/MS) either on triple quadrupole mass spectrometers or on single quadrupoles (by in-source collisional experiments) [6][7][8][9][10][11][12]. Poch et al were the first to propose an LC-MS/MS method in an ion trap (IT) equipped with an atmospheric-pressure chemical ionization (APCI) interface [13] for the determination of O-H-LSD; that method proved suitable for the analysis of the polar metabolite but lacked in specificity for LSD.…”

Section: Introductionmentioning

confidence: 99%

“…1). Because other metabolites which have recently been found in urine at concentrations higher than that of nor-LSD, such as 2-oxo-3-hydroxy-LSD (O-H-LSD), allow detection of LSD consumption in a larger time-window [9,10,13], the method was also able to identify and measure such compounds.…”

Section: Introductionmentioning

confidence: 99%

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LC-ESI-MS/MS on an ion trap for the determination of LSD, iso-LSD, nor-LSD and 2-oxo-3-hydroxy-LSD in blood, urine and vitreous humor

et al. 2006

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A method has been developed for the simultaneous determination of lysergic acid diethylamide (LSD), its epimer iso-LSD, and its main metabolites nor-LSD and 2-oxo-3-hydroxy LSD in blood, urine, and, for the first time, vitreous humor samples. The method is based on liquid/liquid extraction and liquid chromatography-multiple mass spectrometry detection in an ion trap mass spectrometer, in positive ion electrospray ionization conditions. Five microliter of sample are injected and analysis time is 12 min. The method is specific, selective and sensitive, and achieves limits of quantification of 20 pg/ml for both LSD and nor-LSD in blood, urine, and vitreous humor. No significant interfering substance or ion suppression was identified for LSD, iso-LSD, and nor-LSD. The interassay reproducibilities for LSD at 20 pg/ml and 2 ng/ml in urine were 8.3 and 5.6%, respectively. Within-run precision using control samples at 20 pg/ml and 2 ng/ml was 6.9 and 3.9%. Mean recoveries of two concentrations spiked into drug free samples were in the range 60-107% in blood, 50-105% in urine, and 65-105% in vitreous humor. The method was successfully applied to the forensic determination of postmortem LSD levels in the biological fluids of a multi drug abuser; for the first time, LSD could be detected in vitreous humor.

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Section: Ms/msmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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LC-ESI-MS/MS on an ion trap for the determination of LSD, iso-LSD, nor-LSD and 2-oxo-3-hydroxy-LSD in blood, urine and vitreous humor

et al. 2006

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“…Within-and between-day coefficients of variation were 3.5% and 4.0%, respectively, and the extraction recovery was 91%. Canezin et al [73] have developed an HPLC procedure with ESI-MS/MS detection for both urine and blood and validated it for LSD and iso-LSD determination. A one-step liquid-liquid extraction on 1 mL blood or urine was used.…”

Section: Lsdmentioning

confidence: 99%

A critical evaluation of high performance liquid chromatography‐electrospray ionisation‐mass spectrometry and capillary electrophoresis‐ electrospray‐mass spectrometry for the detection and determination of small molecules of significance in clinical and forensic science

Smyth¹,

Brooks

2004

Electrophoresis

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A critical review of applications for the period 2000-2003, taken from the Web of Knowledge database, of the techniques high performance liquid chromatography-electrospray ionisation-mass spectrometry (HPLC-ESI-MS) and capillary electrophoresis-electrospray ionisation-mass spectrometry (CE-ESI-MS) to the detection and determination of small molecules of significance in clinical and forensic science is presented. The molecules of mass less than 500 Da are chosen according to selected structural classes in which they give ESI signals primarily as [M+H](+) ions although other ions such as [M-H](-), [M+Na](+) and [M+NH(4)](+) are also reported. The structural classes are drugs with amine-containing side chains, drugs with N-containing saturated ring structures, 1,4-benzodiazepines, carbohydrates, benzimidazoles, other heterocycles, sulphonylureas, anthracyclines, sulphonamides, penicillins, cephalosporins, tetracyclines, nitrocatechols, steroids, flavonoids, oxazaphosphorines, cannabinols, and miscellaneous molecules. Details are given on the fragmentations, where available, that these ionic species exhibit in-source and in ion-trap, triple quadrupole and time-of-flight mass spectrometers. The review then gives a critical evaluation of these recent HPLC-ESI-MS and CE-ESI-MS analytical methods for the detection and determination of small molecules of clinical and forensic significance. Analytical information on, for example, sample concentration techniques, HPLC and CE separation conditions, recoveries from biological media and limits of detection (LODs) are provided.

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“…Conventional analytical methods used in the last decade consist of liquid chroma- tographic separations with an MS detection following a sample pretreatment step [2]. LSD has been extracted by an alkaline liquid -liquid extraction from urine, blood [3,4], and recently from vitreous humor [5]. SPE was also used for urine samples to provide cleaner extracts with a lowest organic solvent consumption [6,7].…”

Section: Introductionmentioning

confidence: 99%

Selective sample pretreatment by molecularly imprinted polymer for the determination of LSD in biological fluids

Chapuis-Hugon¹,

Cruz-Vera

Savane

et al. 2009

J of Separation Science

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For the first time, a molecularly imprinted polymer (MIP) was synthesized by a noncovalent imprinting approach for the selective extraction of an illicit drug, LSD, from hair and urine samples. For the synthesis of MIP, an analog of LSD, was taken as a dummy template, methacrylic acid as a functional monomer, and ACN as a porogen solvent. The MIP was used for offline extraction before HPLC-MS analysis. By studying the interactions taking place between the LSD and the MIP, a selective procedure was established in organic media and applied to hair samples. By this way, 0.1 ng/mg of LSD was successfully detected in hair with 82% of extraction recovery. A low retention was also obtained on the control polymer (only 9%). This procedure was then modified to obtain a selective extraction in aqueous media for the determination of LSD in urine samples. The comparison with a conventional C18 clearly demonstrated the selectivity brought by the MIP to the determination of LSD in urine. LSD was easily detected in urine at only 0.5 ng/mL with 83% of extraction recovery on the MIP and 11% on the NIP. An LOQ of 0.2 pg/mL was estimated in urine samples.

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Determination of LSD and its metabolites in human biological fluids by high-performance liquid chromatography with electrospray tandem mass spectrometry

Cited by 56 publications

References 20 publications

LC-ESI-MS/MS on an ion trap for the determination of LSD, iso-LSD, nor-LSD and 2-oxo-3-hydroxy-LSD in blood, urine and vitreous humor

LC-ESI-MS/MS on an ion trap for the determination of LSD, iso-LSD, nor-LSD and 2-oxo-3-hydroxy-LSD in blood, urine and vitreous humor

A critical evaluation of high performance liquid chromatography‐electrospray ionisation‐mass spectrometry and capillary electrophoresis‐ electrospray‐mass spectrometry for the detection and determination of small molecules of significance in clinical and forensic science

Selective sample pretreatment by molecularly imprinted polymer for the determination of LSD in biological fluids

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