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Containing 0.1% Formic Acid (containing 0.1% + formic_acid)

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Chemistry100%

Selected Abstracts

Rapid screening and confirmation of drugs and toxic compounds in biological specimens using liquid chromatography/ion trap tandem mass spectrometry and automated library search

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 1 2010
Hsiu-Chuan Liu
Recent advances in liquid chromatography/tandem mass spectrometry (LC/MS/MS) technology have provided an opportunity for the development of more specific approaches to achieve the ,screen' and ,confirmation' goals in a single analytical step. For this purpose, this study adapts the electrospray ionization ion trap LC/MS/MS instrumentation (LC/ESI-MS/MS) for the screening and confirmation of over 800 drugs and toxic compounds in biological specimens. Liquid-liquid and solid-phase extraction protocols were coupled to LC/ESI-MS/MS using a 1.8-µm particle size analytical column operated at 50°C. Gradient elution of the analytes was conducted using a solvent system composed of methanol and water containing 0.1% formic acid. Positive-ion ESI-MS/MS spectra and retention times for each of the 800 drugs and toxic compounds were first established using 1,10,µg/mL standard solutions. This spectra and retention time information was then transferred to the library and searched by the identification algorithm for the confirmation of compounds found in test specimens , based on retention time matches and scores of fit, reverse fit, and purity resulting from the searching process. The established method was found highly effective when applied to the analyses of postmortem specimens (blood, urine, and hair) and external proficiency test samples provided by the College of American Pathology (CAP). The development of this approach has significantly improved the efficiency of our routine laboratory operation that was based on a two-step (immunoassay and GC/MS) approach in the past. Copyright © 2009 John Wiley & Sons, Ltd. [source]

Development and validation of UPLC-MS/MS method for simultaneous determination of gestodene and ethinyl estradiol in rat plasma

BIOMEDICAL CHROMATOGRAPHY, Issue 2 2010
Zhili Xiong
Abstract A selective and sensitive ultra-performance liquid chromatography method with tandem mass spectrometric detection for simultaneous determination of gestodene (GES) and ethinyl estradiol (EE) in rat plasma was developed and validated. GES, EE and the internal standard, norgestrel, were extracted with ethyl acetate, derivatized (EE only) with dansyl chloride and then back-extracted into diethyl ether-hexane (2:1, v/v). The separation was performed on an ACQUITY UPLCÔ BEH C18 column with gradient elution using mobile phase consisting of acetonitrile and water (both containing 0.1% formic acid). The detection was carried out by means of electrospray ionization (ESI) mass spectrometry in positive ion mode with multiple-reaction monitoring. Calibration curves of GES and EE were linear (r2,,,0.99) over the concentration ranges 1.59,159 and 0.196,78.4,ng/mL, respectively. The intra- and inter-day precisions were not more than 6.9 and 12.9% for GES and 10.6 and 9.0% for EE, and the accuracies were ,2.5,8.0% for GES, and ,7.2,0.19% for EE, respectively. The method herein described was superior to previous methods and was applicable to the pharmacokinetic study of GES and EE in rats. Copyright © 2009 John Wiley & Sons, Ltd. [source]

Determination of teniposide in rat plasma by ultra performance liquid chromatography electrospray ionization tandem mass spectrometry after intravenous administration

BIOMEDICAL CHROMATOGRAPHY, Issue 9 2009
Jing Wang
Abstract A novel, specific and rapid ultra performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for determination of teniposide in rat plasma. A one-step liquid,liquid extraction method was used and the separation was carried out on an Acquity UPLCTM BEH C18 column with gradient elution using a mobile phase composed of acetonitrile and water (containing 0.1% formic acid) at a flow rate of 0.20 mL/min. A triple quadrupole tandem mass spectrometer in multiple-reaction monitoring mode via an electrospray ionization interface was used for the detection of teniposide. The detection was complete within 3.0 min. A linear calibration curve was obtained over the concentration range 10,10,000 ng/mL for teniposide, with a lower limit of quantification of 10 ng/mL. The intra-day precision and inter-day precision (relative standard deviation) were less than 10.23 and 13.09%, respectively. The developed method was applied for the first time to the pharmacokinetic study of teniposide in rats following a single intravenous administration of 4.5 mg/kg teniposide. Copyright © 2009 John Wiley & Sons, Ltd. [source]

Simultaneous determination of udenafil and its active metabolite, DA-8164, in human plasma and urine using ultra-performance liquid chromatography,tandem mass spectrometry: application to a pharmacokinetic study

BIOMEDICAL CHROMATOGRAPHY, Issue 9 2008
Soo Kyung Bae
Abstract A rapid, sensitive, and simple ultra-performance liquid chromatography,tandem mass spectrometry (UPLC/MS/MS) method for the determination of udenafil and its active metabolite, DA-8164, in human plasma and urine using sildenafil as an internal standard (IS) was developed and validated. Udenafil, DA-8164 and IS from a 100 µL aliquot of biological samples were extracted by protein precipitation using acetonitrile. Chromatographic separation was carried on an Acquity UPLC BEH C18 column (50 × 2.1 mm, i.d., 1.7 µm) with an isocratic mobile phase consisting of acetonitrile and containing 0.1% formic acid (75:25, v/v) at flow rate of 0.4 mL/min, and total run time was within 1 min. Detection and quantification was performed by the mass spectrometer using multiple reaction-monitoring mode at m/z 517 , 283 for udenafil, m/z 406 , 364 for DA-8164 and m/z 475 , 100 for IS. The assay was linear over a concentration range of 1,600 ng/mL with a lower limit of quantification of 1 ng/mL in both human plasma and urine. The coefficient of variation of this assay precision was less than 13.7%, and the accuracy exceeded 92.0%. This method was successfully applied for pharmacokinetic study after oral administration of udenafil 100 mg to healthy Korean male volunteers. Copyright © 2008 John Wiley & Sons, Ltd. [source]