scholarly journals Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization

2015 ◽  
Vol 65 (2) ◽  
pp. 159-169 ◽  
Author(s):  
Paweł Szpot ◽  
Grzegorz Buszewicz
Keyword(s):  
Electrospray Ionization ◽  
Human Plasma ◽  
Ultra Performance Liquid Chromatography ◽  
High Accuracy ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Flight Mass Spectrometry ◽  
Tof Ms ◽  
Chemical Formulas

Abstract This report presents the application of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry with positive electrospray ionization, to determine ramipril in human plasma. First, the proteins in human plasma were precipitated using acetonitrile, then the supernatant was extracted by ethyl acetate at pH 3 and finally, the extract was analyzed using a UPLC-QTOF- MS system. The method was validated and the coefficient of determination (R2) was > 0.999, the lower limit of quantification (LLOQ) was 0.5 ng mL-1. Precision, recovery and stability were determined for three different concentrations of ramipril. RSD for this method ranged from 3.3 to 8.6 %. The intra-day mean recovery was from 65.3 to 97.3 %. In addition, the fragmentation of ramipril was studied. Due to high resolution of the spectrometer, it was possible to measure fragment masses accurately and determine their molecular and chemical formulas with high accuracy.

Rapid Determination of Sufentanil in Human Plasma by UHPLC–QqQ-MS-MS

2020 ◽  
Author(s):  
Marcin Zawadzki ◽  
Grzegorz Kowalski ◽  
Agnieszka Chłopaś-Konowałek ◽  
Marta Siczek ◽  
Małgorzata Sobieszczańska ◽  
...  
Keyword(s):  
Human Plasma ◽  
Lower Limit ◽  
Rapid Determination ◽  
Ultra Performance Liquid Chromatography ◽  
Sample Volume ◽  
Small Sample ◽  
Plasma Samples ◽  
Limit Of Quantification ◽  
Detection And Identification

Abstract This paper presents a rapid, sensitive and precise method developed and validated for the quantification of sufentanil in biological samples using ultra-performance liquid chromatography coupled with QqQ-MS-MS. Plasma samples were extracted with simple and fast liquid-liquid extraction (ethyl acetate, pH 9). Calibration curve showed linearity in the concentration range of 0.005–30 µg/L. The lower limit of quantification was 0.010 µg/L. The most important method features are low lower limit of quantification value, simple plasma extraction and small sample volume. This method is suitable not only for evaluation of the pharmacokinetics, toxicology, bioavailability and clinical pharmacology of sufentanil but also for the detection and identification of this compound in human plasma samples for forensic purposes.

scholarly journals Column Liquid Chromatography/Electrospray Ionization-Time of Flight-Mass Spectrometry and Ultraperformance Column Liquid Chromatography/Mass Spectrometry Methods for the Determination of Ginkgolides and Bilobalide in the Leaves of Ginkgo biloba and Dietary Supplements

2009 ◽  
Vol 92 (2) ◽  
pp. 645-652 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Troy J Smillie ◽  
Ikhlas A Khan
Keyword(s):  
Mass Spectrometry ◽  
Column Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Electrospray Ionization ◽  
Ginkgo Biloba ◽  
Ionization Time ◽  
Flight Mass Spectrometry ◽  
Tof Ms

Abstract Column liquid chromatography/electrospray ionization-time of flight-mass spectrometry (LC/ESI-TOF-MS) and ultraperformance column liquid chromatographic/MS (UPLC/MS) methods were developed for the determination of 5 terpenelactones in the leaves of Ginkgo biloba. The separation was performed using a C18 column and a mobile phase composed of water and acetonitrile. The limit of detection (LOD) values for ginkgolide J, ginkgolide C, ginkgolide B, and ginkgolide A were found to be in the range of 110 ng/mL by both methods, and the bilobalide LOD was 200 ng/mL by LC/ESI-TOF and 35 ng/mL by UPLC/MS. Using the optimized method, 4 commercial products were analyzed. Concentrations of total marker compounds in these products were in the 0.0915.4 range, with individual ginkgo terpenelactones being detected at ppb levels. LC/MS with ESI is described for the identification and quantification of ginkgolides and bilobalide in plant samples and dietary supplements that claim to contain G. biloba. These methods involve the use of the M NH4<sup/> and M H<sup/> ions of sesquiterpenoids in the positive ion mode with extractive ion monitoring by LC/ESI-TOF-MS and selected ion monitoring by UPLC/MS. The LC method coupled with MS analysis yielded well-separated peaks which resulted in a clear identification of the compounds.

scholarly journals Determination of Progestin Residues in Fish by UPLC-Q-TOF/MS Coupled with QuEChERS

2019 ◽  
Vol 2019 ◽  
pp. 1-6
Author(s):  
Chunxiu Gu ◽  
Yanling Cheng ◽  
Xin Zhen ◽  
Xiaoxuan Chen ◽  
Kaowen Zhou
Keyword(s):  
Ultra Performance Liquid Chromatography ◽  
Technical Support ◽  
Quantitative Detection ◽  
Quechers Method ◽  
Aquatic Products ◽  
Flight Mass Spectrometry ◽  
Relative Standard ◽  
Novel Method ◽  
Tof Ms

A novel method was developed for simultaneous determination of 10 progestin residues in fish by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS) combined with a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The homogenized samples were dispersed by water, extracted with acetonitrile, and then purified by QuEChERS reagent. The concentrated analytes were detected by UPLC-Q-TOF/MS. High linearities (R2 > 0.995) and recoveries (85.71–117.08%) at three spiked levels (5, 10, and 20 ng/g) and low relative standard deviation values (<8.83%, n = 7) and limits of detection (0.23–0.66 ng/g) were obtained. This method is simple, rapid, reliable, sensitive, and efficient and can be used for monitoring of progestin residues in fish. This method provides a strong guarantee to deal with food emergencies for the laboratory, provides technical support for the screening and quantitative detection of progesterone in fish, and provides technical support for the food safety of aquatic products.

scholarly journals Determination of Flavonoid Glycosides by UPLC-MS to Authenticate Commercial Lemonade

Molecules ◽  
2019 ◽  
Vol 24 (16) ◽  
pp. 3016 ◽  
Author(s):  
Ying Xue ◽  
Lin-Sen Qing ◽  
Li Yong ◽  
Xian-Shun Xu ◽  
Bin Hu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Low Cost ◽  
Ultra Performance Liquid Chromatography ◽  
Flavonoid Glycosides ◽  
Molecular Formula ◽  
Flight Mass Spectrometry ◽  
Dispersive Liquid Liquid Microextraction ◽  
Tof Ms

So far, there is no report on the quality evaluation of lemonade available in the market. In this study, a sample preparation method was developed for the determination of flavonoid glycosides by ultra-performance liquid chromatography–mass spectrometry (UPLC-MS) based on vortex-assisted dispersive liquid-liquid microextraction. First, potential flavonoids in lemonade were scanned and identified by ultra-performance liquid chromatography–time of flight mass spectrometry (UPLC-TOF/MS). Five flavonoid glycosides were identified as eriocitrin, narirutin, hesperidin, rutin, and diosmin according to the molecular formula provided by TOF/MS and subsequent confirmation of the authentic standard. Then, an ultra-performance liquid chromatography–triple quadrupole mass spectrometry (UPLC-QqQ/MS) method was developed to determine these five flavonoid glycosides in lemonade. The results showed that the content of rutin in some lemonade was unreasonably high. We suspected that many illegal manufacturers achieved the goal of low-cost counterfeiting lemonade by adding rutin. This suggested that it was necessary for relevant departments of the state to make stricter regulations on the quality standards of lemonade beverages.

scholarly journals Determination of 35 Free Amino Acids in Tea Using Ultra-Performance Liquid Chromatography Coupled With Quadrupole Time-of-Flight Mass Spectrometry

2021 ◽  
Vol 8 ◽  
Author(s):  
Jian Li ◽  
Junmei Ma ◽  
Qiang Li ◽  
Sufang Fan ◽  
Lixin Fan ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Amino Acids ◽  
Liquid Chromatography ◽  
Free Amino Acids ◽  
Free Amino ◽  
Time Of Flight ◽  
Ultra Performance Liquid Chromatography ◽  
Flight Mass Spectrometry ◽  
Tof Ms

The purpose of this research was to develop a simple, sensitive, and accurate method for simultaneous determination of 35 free amino acids using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Tea samples were extracted with boiling water bath, and then separated by XBridge BEH Amide column by gradient elution. The exact mass and MS/MS spectra of the target compound was detected under the TOF–MS and Information dependent acquisition (IDA)–MS/MS mode. The results demonstrated good linearity (R2 &gt; 0.9980) in the range of 0.5–1,000 ng/mL. The limits of detection (LODs) were 0.13–25.00 mg/kg and the limits of quantitation (LOQs) were 0.25–50.00 mg/kg. The recovery rate ranged from 70.1 to 105.1% with relative standard deviations (RSDs) &lt;11% (n = 6). This research provides a targeted strategy for developing an analysis method for amino acids in tea.

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