The effects of sample preparation methods on the variability of the electrospray ionization response for model drug compounds

Bonfiglio, Ryan; King, Richard C.; Olah, Timothy; Merkle, Kara

doi:10.1002/(sici)1097-0231(19990630)13:12<1175::aid-rcm639>3.0.co;2-0

Cited by 890 publications

(623 citation statements)

References 17 publications

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“…Several methods could be used to determine whether sample matrix affects performance of a method (Bonfiglio et al, 1999;King et al, 2000;Matuszewski, Constanzer, & Chavez-Eng, 2003;Kaufmann and Butcher, 2005). Common approach to evaluate ion suppression is with post-column infusion of the target analyte in the effluent from the chromatographic column, while analyzing patient samples (Kaufmann & Butcher, 2005).…”

Section: Lc-ms/ms In Clinical Diagnosticsmentioning

confidence: 99%

Liquid chromatography-tandem mass spectrometry applications in endocrinology

Kushnir

Rockwood

Bergquist

2009

Mass Spectrom. Rev.

139

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Liquid chromatography-tandem mass spectrometry (LC-MS/ MS) has been recognized as a primary methodology for the accurate analysis of endogenous steroid hormones in biological samples. This review focuses on the use of LC-MS/MS in clinical laboratories to assist with the diagnosis of diverse groups of endocrine and metabolic diseases. Described analytical methods use on-line and off-line sample preparation and analytical derivatization to enhance analytical sensitivity, specificity, and clinical utility. Advantages of LC-MS/MS as an analytical technique include high specificity, possibility to simultaneously measure multiple analytes, and the ability to assess the specificity of the analysis in every sample. All described analytical methods were extensively validated, utilized in routine diagnostic practice, and were applied in a number of clinical and epidemiological studies, including a study of the steroidogenesis in ovarian follicles. #

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Section: Lc-ms/ms In Clinical Diagnosticsmentioning

confidence: 99%

Liquid chromatography-tandem mass spectrometry applications in endocrinology

Kushnir

Rockwood

Bergquist

2009

Mass Spectrom. Rev.

139

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“…Selectivity was confirmed using multiple sourced and pooled blank brain samples as well as injecting other controlled substances into the assay and monitoring for interference on the direct MS/MS channels for each analyte and internal standard. Regions of ionization suppression were determined using a post-column infusion of the drug standards in methanol while simultaneously injecting an extracted blank brain sample through the analytical column (34). The blank brain sample showed a distinct ionization suppression region from 0.5 to 1.75 min, but this precedes the elution of the synthetic cathinones or their corresponding internal standards.…”

Section: Methods Developmentmentioning

confidence: 99%

“…Regions of ionization suppression associated with the brain tissue matrix were determined using the post-column infusion experiment pioneered by Bonfiglio et al (34). Blank brain homogenate was prepared as indicated above and injected onto the analytical column while methanolic solutions of the analytes and internal standards (1 μg/mL) were infused into the electrospray source using a Harvard Apparatus Pump 11+ (Holliston, MA) through a solvent mixing tee.…”

Section: Selectivity and Ionization Suppressionmentioning

confidence: 99%

Quantification of Synthetic Cathinones in Rat Brain Using HILIC–ESI-MS/MS

et al. 2016

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The abuse of synthetic cathinones, formerly marketed as "bath salts", has emerged over the last decade. Three common drugs in this class include 3,4-methylenedioxypyrovalerone (MDPV), 4-methylmethcathinone (mephedrone), and 3,4-methylenedioxymethcathinone (methylone). An LC-MS/MS method has been developed and validated for the simultaneous quantification of MDPV, mephedrone, and methylone in brain tissue. Briefly, MDPV, mephedrone, methylone, and their deuterium-labeled analogs were subjected to solid phase extraction (SPE) and separated using an HILIC Silica Column. The HPLC was coupled to a Shimadzu IT-TOF (ion trap-time of flight) system with the electrospray source running in positive mode (+ESI). The method was validated for precision, accuracy, and extraction efficiency. All inter-day and intra-day % RSD (percent relative standard deviation) and % error values were less than 15% and extraction efficiency exceeded 80%. These conditions allowed for limits of detection of 1ng/mL for MDPV, and 5 ng/mL for both mephedrone and methylone. The limits of quantification were determined to be 5ng/mL for MDPV and 10 ng/mL for mephedrone and methylone. The method was utilized to evaluate the pharmacokinetics of these drugs in adult male rats following administration of a drug cocktail including MDPV, mephedrone, and methylone. All three compounds reached peak concentrations in the brain within 15 min. Although methylone and mephedrone were administered at the same dose, the peak concentration (C max ) of mephedrone in the brain was significantly higher than that for methylone, as was the area under the curve (AUC). In summary, this quick and sensitive method for measuring synthetic cathinones may be used for future pharmacokinetic investigations of these drugs in target tissue.

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“…Matrix effect was evaluated by post-column analyte infusion experiments based on method described by Bonfiglio et al 29 Four different blank plasma sample (including normal, lipemic and hemolysed) were extracted under on-line SPE conditions and chromatographed. No significant ion suppression effect was observed in codeine and IS retention time.…”

Section: Methods Validationmentioning

confidence: 99%

On-line solid phase extraction coupled with liquid chromatography tandem mass spectrometry for the determination of codeine in human plasma

Cruz

Suenaga

Abib³

et al. 2016

Quim. Nova

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publicado na web em 26/08/2016A specific LC-MS/MS method was developed and validated for automated determination of codeine in human plasma, using online solid phase extraction (SPE) system coupled with positive ion electrospray ionization tandem mass spectrometry. The method allowed plasma direct injection onto cartridge without sample pre-treatment. Total analysis time per run was 3 min, allowing highthroughput for codeine determination. SPE on-line along a monolithic column (Chromolith Performance RP-18e, 100 mm x 4.6 mm) demonstrated to be highly effective in terms of backpressure, separation speed and peak asymmetry. Calibration curves range was linear 5.0-200 ng mL -1 . Method showed an excellent intra-day and inter-day precision ranged from 2.34 to 7.25% (CV%) as well as great intra-day and inter-day accuracy, ranging from 97.64 to 110% (RE%). SPE-LC-MS/MS method provided selectivity, accuracy, precision, fastness and high-throughput to assess codeine pharmacokinetics in human plasma samples.

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The effects of sample preparation methods on the variability of the electrospray ionization response for model drug compounds

Cited by 890 publications

References 17 publications

Liquid chromatography-tandem mass spectrometry applications in endocrinology

Liquid chromatography-tandem mass spectrometry applications in endocrinology

Quantification of Synthetic Cathinones in Rat Brain Using HILIC–ESI-MS/MS

On-line solid phase extraction coupled with liquid chromatography tandem mass spectrometry for the determination of codeine in human plasma

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