scholarly journals Simultaneous mass detection for direct inlet mass spectrometry

1979 ◽  
Author(s):  
R.L. Gordon
2018 ◽  
Vol 10 (4) ◽  
pp. 87
Author(s):  
Yahdiana Harahap ◽  
Norma Andriyani ◽  
Harmita .

Objective: To obtain an optimum and validated method for analyzing lercanidipine in plasma using Ultra Performance Liquid Chromatography of Tandem Mass Spectrometry (UPLC-MS/MS).Methods: The separation was carried out using 1.7μm (2.1 x 100 mm) Waters AcquityTM UPLC C18 column, a mobile phase of the 0.1% formic acid-methanol mixture (20:80 v/v) with isocratic elution, 30 °C column temperature, 0.2 ml/min flow rate and amlodipine as an internal standard. Mass detection was performed with a positive XBL TQD type Electrospray Ionization (ESI) in Multiple Reaction Monitoring modes. Lercanidipine was detected at m/z value of 612.11>280.27 and amlodipine was detected at m/z value 409.1>238.15. The optimum sample preparation method was a liquid-liquid extraction using 5 ml of n-hexane-ethyl acetate (50:50 v/v), vortex mixed for 3 min, centrifuged at 4000 rpm for 20 min, evaporated with nitrogen at 50 °C for 30 min, and the residue was reconstituted with 100 μl of mobile phase.Results: The method was linear in the range of 0.025-10 ng/ml with r ≥ 0.9986. Accuracy and precision within-run and between-run met the requirements with %diff and %CV, not exceeding ± 15% and not more than ± 20% for Lower Limit of Quantification (LLOQ) concentration.Conclusion: It was concluded that the developed method met the requirements of selectivity, carry over, stability, the integrity of dilution, and matrix effects under the Guideline on Bioanalytical Method Validation by the European Medicines Agency in 2011. 


Molecules ◽  
2019 ◽  
Vol 24 (2) ◽  
pp. 233 ◽  
Author(s):  
Huanyu Guan ◽  
Xiaomei Luo ◽  
Xiaoyan Chang ◽  
Meifeng Su ◽  
Zhuangzhuang Li ◽  
...  

Wen Luo Yin (WLY), a well-known traditional Chinese medicine formulation, has been used as a complementary therapy for the treatment of rheumatoid arthritis in clinical settings. However, the chemical constituents of WLY remain unclear. In this study, a high-performance liquid chromatography coupled with tandem mass spectrometry method was established to separate and comprehensively identify the chemical constituents of WLY. The analytes were eluted with a mobile phase of acetonitrile and 0.1% aqueous acetic acid. Mass detection was performed in both positive and negative ion mode. The MS/MS fragmentation pathways were proposed for the identification of the components. A total of 42 compounds including sesquiterpenes, alkaloids, biflavonoids, polyacetylenes, phenylpropanoids and acetylenic phenols were identified unambiguously or tentatively according to their retention times and mass behavior with those of authentic standards or literature data. The identification and structural elucidation of chemical constituents may provide important information for quality control and pharmacological research of WLY.


2016 ◽  
Vol 62 (1) ◽  
pp. 134-143 ◽  
Author(s):  
Mark W Duncan ◽  
Dobrin Nedelkov ◽  
Ryan Walsh ◽  
Stephen J Hattan

Abstract BACKGROUND MALDI-TOF mass spectrometry (MS) is set to make inroads into clinical chemistry because it offers advantages over other analytical platforms. These advantages include low acquisition and operating costs, ease of use, ruggedness, and high throughput. When coupled with innovative front-end strategies and applied to important clinical problems, it can deliver rapid, sensitive, and cost-effective assays. CONTENT This review describes the general principles of MALDI-TOF MS, highlights the unique features of the platform, and discusses some practical methods based upon it. There is substantial potential for MALDI-TOF MS to make further inroads into clinical chemistry because of the selectivity of mass detection and its ability to independently quantify proteoforms. SUMMARY MALDI-TOF MS has already transformed the practice of clinical microbiology and this review illustrates how and why it is now set to play an increasingly important role in in vitro diagnostics in particular, and clinical chemistry in general.


2007 ◽  
Vol 18 (4) ◽  
pp. 600-606 ◽  
Author(s):  
Oscar Yanes ◽  
Francesc X. Avilés ◽  
Ryan Wenzel ◽  
Alexis Nazabal ◽  
Renato Zenobi ◽  
...  

2007 ◽  
Vol 53 (2) ◽  
pp. 300-309 ◽  
Author(s):  
Elisabeth Leere Øiestad ◽  
Unni Johansen ◽  
Asbjorg Solberg Christophersen

Abstract Background: Oral fluid is an alternative matrix with potential applications in road-side drug screening, work-place testing, drug treatment programs, and epidemiological surveys. Development of methods for extensive drug screening in oral fluid is warranted. Methods: We developed a liquid chromatography– tandem mass spectrometry (LC-MS/MS) method for drug screening of preserved oral fluid collected with the Intercept® collection device. Samples were prepared by liquid–liquid extraction with ethylacetate/heptane (4:1). LC-separation was achieved with an Atlantis dC18-column (2.1 × 50 mm, 3 μm particle). Mass detection was performed by positive ion mode electrospray LC-MS/MS and included the following drugs/metabolites: morphine, 6-monoacetylmorphine, codeine, buprenorphine, methadone, amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxyethylamphetamine, cocaine, benzoylecgonine, Δ-9-tetrahydrocannabinol, lysergic acid diethylamide, alprazolam, bromazepam, clonazepam, 7-aminoclonazepam, diazepam, N-desmethyldiazepam, 3-OH-diazepam, fenazepam, flunitrazepam, 7-aminoflunitrazepam, lorazepam, nitrazepam, 7-aminonitrazepam, oxazepam, zopiclone, zolpidem, carisoprodol, and meprobamat. Results: Screening of 32 drugs was performed with a run time of 14 min. Within- and between-day relative CVs varied from 2.0% to 31.8% and from 3.6% to 39.1%, respectively. Extraction recoveries were >50% except for morphine (30%) and benzoylecgonine (0.2%). The concentrations of the lowest calibrator were 1 nmol/L (0.28 μg/L) to 500 nmol/L (68 μg/L), depending on the drug. Conclusion: The method allowed rapid and sensitive oral fluid screening for the most commonly abused drugs in Norway and will be used for a road-side survey of drug use in normal traffic.


Radiocarbon ◽  
2010 ◽  
Vol 52 (3) ◽  
pp. 1270-1276 ◽  
Author(s):  
J Genberg ◽  
K Stenström ◽  
M Elfman ◽  
M Olsson

To be able to successfully measure radiocarbon with accelerator mass spectrometry (AMS) in atmospheric aerosol samples, graphitization of small sample sizes (<50 μg carbon) must provide reproducible results. At Lund University, a graphitization line optimized for small samples has been constructed. Attention has been given to minimize the reduction reactor volume and each reactor is equipped with a very small pressure transducer that enables constant monitoring of the reaction. Samples as small as 25 μg of carbon have been successfully analyzed, and the mass detection limit of the system has probably not been reached.


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