A Solid Phase Extraction Method for Determination of Nicotine in Serum and Urine by Isotope Dilution Gas Chromatography/Mass Spectrometry with Selected Ion Monitoring

1998 ◽  
Vol 35 (4) ◽  
pp. 522-527 ◽  
Author(s):  
Leland B Baskin ◽  
Rodger W Anderson ◽  
Joel R Charlson ◽  
Richard D Hurt ◽  
George M Lawson
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Nicotine Concentration ◽  
Transdermal Nicotine ◽  
Serum And Urine

A rapid method for measuring nicotine concentration in serum and urine is described. Deuterated nicotine is used as an internal standard. Nicotine and deuterated nicotine are extracted using a copolymeric-bonded phase silica column. The extract is analysed by gas chromatography coupled with mass spectrometry (GC/MS) operating in selected ion monitoring mode. The method has a lower limit of detection of approximately 2 μg/L and is linear to at least 2000 μg/L. Within-run percentage coefficients of variation (% CV) are < 4 in both assays over a nicotine concentration range of 10–2000 μg/L. Between-run %CV in the serum assay are 5.4, 5.2, 4.8 and 5.9, respectively, at nicotine concentrations of 10, 15, 25, and 50 μg/L. Between-run %CV in the urine assay are 5.9, 4.5, 2.7 and 5.2, respectively, at nicotine concentrations of 100, 250, 500, and 2000 μg/L. The absolute recovery of nicotine is 61±+6% (mean±SD) over the range of 10–250 μg/L. The assay has been used to measure serum nicotine concentrations and 24-h urinary excretion of nicotine to monitor the extent of replacement in subjects receiving transdermal nicotine therapy for smoking cessation.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

scholarly journals Development of Sensitive and Specific Analysis of Vildagliptin in Pharmaceutical Formulation by Gas Chromatography-Mass Spectrometry

2015 ◽  
Vol 2015 ◽  
pp. 1-7
Author(s):  
Ebru Uçaktürk
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Pharmaceutical Formulation ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Validation Parameters ◽  
Diagnostic Ions

A sensitive and selective gas chromatography-mass spectrometry (GC-MS) method was developed and fully validated for the determination of vildagliptin (VIL) in pharmaceutical formulation. Prior to GC-MS analysis, VIL was efficiently derivatized with MSTFA/NH4I/β-mercaptoethanol at 60°C for 30 min. The obtained O-TMS derivative of VIL was detected by selected ion monitoring mode using the diagnostic ionsm/z223 and 252. Nandrolone was chosen as internal standard. The GC-MS method was fully validated by the following validation parameters: limit of detection (LOD) and quantitation (LOQ), linearity, precision, accuracy, specificity, stability, robustness, and ruggedness. LOD and LOQ were found to be 1.5 and 3.5 ng mL−1, respectively. The GC-MS method is linear in the range of 3.5–300 ng mL−1. The intra- and interday precision values were less than ≤3.62%. The intra- and interday accuracy values were found in the range of-0.26–2.06%. Finally, the GC-MS method was successfully applied to determine VIL in pharmaceutical formulation.

scholarly journals Simultaneous Quantification of the New Psychoactive Substances 3-FMC, 3-FPM, 4-CEC, and 4-BMC in Human Blood using GC-MS

2019 ◽  
Vol 17 (1) ◽  
pp. 902-911
Author(s):  
Abdulsallam Bakdash
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Human Blood ◽  
Solid Phase ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
New Psychoactive Substances ◽  
Selected Ion Monitoring ◽  
Simultaneous Quantification ◽  
Chromatography Mass Spectrometry

AbstractA gas chromatography-mass spectrometry (GC-MS) method for simultaneous quantification of 3-fluoromethcathinone (3-FMC), (±)-3-fluorophenmetrazine (3-FPM), 4-chloroethcathinone (4-CEC) and 4-Bromomethcathinone (4-BMC) in human blood with (±)-methcathinone-D3 as internal standard has been developed and validated. Whole blood samples were treated with 10% trichloroacetic acid for protein precipitation before solid phase extraction. The method was selective, the calibration curves showed linearity for all substances with R2 ranging from 0.991 to 0.998 in the range 5-1.000 ng/mL. Analysis of blank samples showed no-sign of carryover. Precision and accuracy were acceptable with values less than 20% (RSD) and ± 20% (Bias). The limit of quantification (LOQ) for all substances was 5ng/mL. Intra-day and inter-day precision were 2.111.7% and 1.3 -10.2% respectively and accuracy biases were between -10.6-19.6% % (intra-day) and 11-12.1% (inter-day). The extraction efficiencies were 85.4, 82.8, 79.1 and 74.9% for 3-FMC, 3-FPM, 4-CEC and 4-BMC respectively.A robust and reliable simultaneous quantification method using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS-SIM) is reported.

The Determination of Eight Pesticides in Panax notoginseng of Chinese Traditional Medicine Using Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 485 ◽  
pp. 68-71
Author(s):  
Na Wu ◽  
Yu Da Zhang ◽  
Wei Liu ◽  
Ping Yi ◽  
Ze Feng Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Panax Notoginseng ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A simple and effective extraction method based on solid-phase extraction (SPE) was developed to determine chlorothalonil, metalaxyl, triadimefon, dimetachlone, procymidone, flumetralin, oxadixyl and iprodione in Panax Notoginseng using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS, SIM). The prepared samples were analysed with GC-MS in the selected ion monitoring mode (SIM) using one target and two or three qualitative ions for each analyte. In the method, hexane - dichloromethane（6:4，v/v）was selected to effectively extract the pesticides from the Panax Notoginseng samples. Solid-phase extraction was carried out using Supelclean ENVI-Carb/NH2 SPE Column with acetonitrile-toluene (3:1, v/v) as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R2≥0.99. The limit of detection ranged from 0.001 to 0.05 µg.mL-1, average recoveries ranged from 79.80% to 95.00%, with relative standard deviations between 1.96% and 4.32% for all 8 pesticides.They were readily achieved with this method for all tested pesticides.

Postmortem Analysis of Benzodiazepines in Human Bone by Gas Chromatography–Mass Spectrometry

2020 ◽  
Author(s):  
Rosanna Mancini ◽  
Lucia Fernadez-Lopez ◽  
Maria Falcon ◽  
Manuela Pellegrini ◽  
Aurelio Luna ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Fused Silica ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Fused Silica Capillary ◽  
Silica Capillary Column

Abstract A procedure based on gas chromatography-mass spectrometry was developed for the analysis of benzodiazepines (nordiazepam, oxazepam, lormetazepam, lorazepam, clonazepam, bromazepam and alprazolam) in postmortem human ribs. Powdered bone samples, including marrow remains inside, with the internal standard diazepam-d5 were subjected to enzymatic hydrolysis with 100 μL of β-glucoronidase and were incubated in sodium hydroxide for 1 h in a 70°C oven. Samples underwent liquid phase extraction and ethyl acetate was used as eluent. Chromatography was performed on a fused silica capillary column and the selected-ion-monitoring mode was used for analytes determination. The method was validated in the range 0.1–0.5 ng/mg (depending on the benzodiazepine) to 100 ng/mg with average values of recovery, matrix effect and process efficiency ranged from 83.2 to 94.3%, from 97.3 to 102.1% and from 80.5 to 91.2%, respectively. The intra- and inter-day accuracy was &lt;15%. The procedure was tested in rib specimens obtained during routine autopsies from 20 cases where these benzodiazepines were found in blood. Benzodiazepines were detected in the combined bone and marrow samples in 60% of cases. Lorazepam was detected in bone in the range of 0.3–0.7 ng/mg, nordiazepam at 1.3–4.2 ng/mg and oxazepam at 1.1–1.2 ng/mg. To our knowledge, this protocol for the simultaneous analysis of these benzodiazepines is the first performed and validated using human ribs.

Simultaneous Analysis of Simple Coumarins and Furocoumarines in Cigarettes by Solid-Phase Extraction with Gas Chromatography-Mass Spectrometry

2017 ◽  
Vol 100 (5) ◽  
pp. 1559-1564 ◽  
Author(s):  
Yang Zheng ◽  
Xiuli Xu ◽  
Fei Yuan ◽  
Meiyi Yao ◽  
Shunli Ji ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Oasis Hlb ◽  
Coumarin 6

Abstract A sensitive, high-throughput analytical method based on a GC-MS method was established for the simultaneous quantitative determination of two categories of harmful coumarins: simple coumarins (coumarin, 6-methylcoumarin, 7-methoxycoumarin, 3,4-dihydrocoumarin, and 7-ethoxy-4-methylcoumarin) and furocoumarines (psoralen, 8-methoxypsoralen, 5-methoxypsoralen, and trioxysalen). The nine analytes were extracted with ethyl acetate, purified with Oasis HLB solid-phase extraction (SPE) cartridges, and identified and quantitatively determined by GC-MS in selected-ion monitoring mode. The LODs and LOQs of these compounds were in the ranges of 12.5–21.2 and 41.6–70.0 μg/kg, respectively. Average recoveries for the nine analytes ranged from 72.7 to 86.6% atLOQ, 1.5× LOQ, and 2× LOQ spike levels, with RSDs that were typically lower than 5.1%. TheSPE-GC-MS method developed in this study was initially applied to research coumarins in cigarette samples; it proved to be accurate, sensitive, convenient, and practical.

scholarly journals A Novel Application of Natural Peat for Solid-Phase Extraction of Pyrimethanil, Flumetralin, and Kresoxim-Methyl in Water Using Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 2012 ◽  
pp. 1-5
Author(s):  
Alex S. M. S. J. Santos ◽  
Adriano Aquino ◽  
Luciane P. C. Romão ◽  
Sandro Navickiene
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Detection And Quantification

Natural peat was tested for extraction of pyrimethanil, flumetralin, and krexosim-methyl from water, with analysis using gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Experiments were carried out at one fortification level (0.1 μg L−1) and resulted in recoveries in the range 41–96%, with RSD values between 6.8 and 12.6% for natural peat as sorbent. Detection and quantification limits ranged from 0.02 to 0.05 μg L−1 and from 0.07 to 0.1 μg L−1, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.07–4.0 μg L−1), with correlation coefficients ranging from 0.9919 to 0.9989. Comparison between peat and commercial sorbents (C18-bonded silica, ENVI-Carb, Florisil, silica gel, ENVI-Carb/LC-NH2) showed better performance of peat sorbent for flumetralin and kresoxim-methyl.

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