On-Line Immunoaffinity Extraction-Coupled Column Capillary Liquid Chromatography/Tandem Mass Spectrometry:  Trace Analysis of LSD Analogs and Metabolites in Human Urine

Cai, Jianyi; Henion, Jack D.

doi:10.1021/ac950763i

Cited by 108 publications

(46 citation statements)

References 39 publications

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“…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%

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: Introductionmentioning

confidence: 99%

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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“…The most recent applications of pre-column immunoextraction include immunoextraction/HPLC/mass spectrometroscopy for determination of corticosteroids including dexamethasone and flumethasone in post administration equine urine samples (Creaser et al, 1998), confirmation analysis of clenbuterol in beef liver and minced beef (Lau et al, 1997), quantitative multiresidue determination of b-agonists in bovine urine (Cai and Henion, 1997), trace analysis of LSD analogs and metabolites in human urine (Cai and Henion, 1996), analysis of pesticide degradation products (Rollag et al, 1996) and determination of carbofuran (Rule et al, 1994). The application of mass spectrometry in on-line pre-column immunodetection can provide detection of multiple compounds in one assay.…”

Section: Pre-column Immunoassays Coupled To Lcmentioning

confidence: 99%

Coupling immunoassays with chromatographic separation techniques

Tang

Karnes

2000

Biomed. Chromatogr.

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Coupling immunoassays with HPLC separation techniques is becoming increasingly useful in the analysis of biological and nonbiological samples of both large and small molecules. This is because it provides both sensitivity and selectivity for molecular analysis at relatively low cost, low maintenance and with excellent potential for automation. This paper reviews application of this hyphenated approach both in the pre-column immunoextraction and post-column immunodetection modes. Systems in which immunoassays are interfaced to chromatographic separations in order to separate bound and free fractions of the immunoassay will not be included since these systems do not provide the enhanced selectivity common to hyphenated systems. Post-column immunodetection is based on various immunoassay formats such as direct detection, one-site, competitive and sandwich immunoassays. Homogeneous immunodetectors are more convenient than heterogeneous immunodectors since there are no separation and column regeneration steps involved in homogeneous immunoassays. On the other hand, heterogeneous immunoassays are generally more sensitive than homogeneous immunoassays since interfering substances are removed prior to immunodetection. Advantages and limitations for the various approaches will be discussed.

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“…Such techniques have been demonstrated for the analysis LSD analogs and metabolites in urine. 36,37 They allow clean-up with no precolumn sample preparation and direct quantitation by MS methods.…”

Section: Analysis Of Peptides In Physiological Fluidsmentioning

confidence: 99%

Mass Spectrometry in Pharmaceutical Analysis

Gale¹,

Guiles

Crowther

2000

Encyclopedia of Analytical Chemistry

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Mass spectrometry (MS) applied to the biological sciences in the pharmaceutical industry covers a broad range of application topics, such as quantitative analysis of drugs in physiological fluids, qualitative analysis of noncovalent complexes, structural analysis to determine chirality and protein sequence analysis. Regardless of the application, electrospray ionization (ESI) is the primary ionization method for transfer of nonvolatile biologics like proteins and peptides into the gas phase for analysis. It is most often used as an interface between high‐performance liquid chromatography (HPLC) separation methods and MS. The ESI process converts analytes in solution to ions in the gas phase via electrostatic nebulization at atmospheric pressure. It is characteristic of ESI to produce multiply charged analytes in a concentration‐dependent manner that is sensitive to changes in solvent, pH and ionic strength. A high voltage is applied to a liquid containing analytes as they traverse a capillary, and when the liquid droplets exit this capillary at atmospheric pressure they are directed into the source region of a mass spectrometer where desolvation is completed. Ions are then focused by an electronic gradient across a series of lenses and separated by mass/charge ( m / z ) using various mass spectrometer designs. Currently, the two most popular mass separation devices are quadrupoles (either single or triple quadrupole (TQ)) and ion traps (ITs). Both types of mass spectrometers are used with ESI to achieve sensitivities as low as attomoles (10 −18 mol) of analyte injected onto a microcapillary HPLC column. The type of analyte, as long as it is capable of accepting a charge (addition of H + or loss of charge in negative ion mode) is relatively transparent to ESI and so a diverse range of analyte classes with disparate molecular weights can be ionized, from peptides (500–5000 amu) to proteins (10 000–100 000 amu). Depending on the construction of the source, ESI can be carried out with reversed‐phase HPLC at flow rates from 200 nL min −1 to 2 mL min −1 and also with capillary electrophoresis. The ease of use of ESI compared to prior techniques like fast atom bombardment has made it very popular with biologists, chromatographers and chemists who might not otherwise have been interested in MS. In fact, for many scientists ESI has made MS almost as “user‐friendly” and thus accessible as an ultraviolet (UV)–visible detector for HPLC.

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On-Line Immunoaffinity Extraction-Coupled Column Capillary Liquid Chromatography/Tandem Mass Spectrometry: Trace Analysis of LSD Analogs and Metabolites in Human Urine

Cited by 108 publications

References 39 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

Coupling immunoassays with chromatographic separation techniques

Mass Spectrometry in Pharmaceutical Analysis

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