European journal of mass spectrometry (Chichester, England)最新文献

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Liquid chromatography-tandem mass spectrometry method for quantification of ertugliflozin in human plasma: Application to disposition kinetics. 液相色谱-串联质谱法定量人血浆中厄图格列净:在处置动力学中的应用。
European journal of mass spectrometry (Chichester, England) Pub Date : 2025-07-15 DOI: 10.1177/14690667251359789
Viritha Bezawada, Padma Mogili, Sireesha Dodda, Srinivasa Rao Polagani
{"title":"Liquid chromatography-tandem mass spectrometry method for quantification of ertugliflozin in human plasma: Application to disposition kinetics.","authors":"Viritha Bezawada, Padma Mogili, Sireesha Dodda, Srinivasa Rao Polagani","doi":"10.1177/14690667251359789","DOIUrl":"https://doi.org/10.1177/14690667251359789","url":null,"abstract":"<p><p>A high-performance liquid chromatography-tandem mass spectrometry method has been developed for the quantification of ertugliflozin in human plasma, employing ertugliflozin D5 as the internal standard. Methyl tertiary butyl ether-based liquid-liquid extraction technique was employed, followed by chromatographic separation on Kromasil-C<sub>18</sub> (100 × 4.6 mm, 5 µm) column using a mixture of methanol and 10 mM ammonium formate buffer (80:20, v/v) as the mobile phase at a flow rate of 1 mL/min. The mass transitions were observed from <i>m</i>/<i>z</i> 437.4 to 329.2 for ertugliflozin and from <i>m</i>/<i>z</i> 442.2 to 334.3 for ertugliflozin D5 by multiple reaction monitoring in a positive ion electro spray ionization source. The linearity was established in the concentration range of 1-500 ng/mL, with the correlation coefficient, <i>r</i><sup>2</sup> <b>></b> 0.99. Validation of the method was performed as per US FDA guidelines, and the results were found well within the acceptance limits. The method was applied successfully for the pharmacokinetic study of ertugliflozin 15 mg after a single oral dose under fasting conditions in healthy male volunteers. The <i>C</i><sub>max</sub> and <i>t</i><sub>max</sub> values obtained were 288.28 ng/mL and 1.32 h, respectively. Authentication of the results was further done by the incurred sample reanalysis.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"14690667251359789"},"PeriodicalIF":0.0,"publicationDate":"2025-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144639495","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of kinetic characteristics of thermal desorption of cocaine by mass-spectrometric method of surface ionization. 表面电离质谱法测定可卡因热解吸动力学特性。
European journal of mass spectrometry (Chichester, England) Pub Date : 2025-07-11 DOI: 10.1177/14690667251358340
Ganiboy T Rakhmanov, Tursunali S Kholikov, Azim Sh Radjabov, Saida S Iskhakova, Dilshadbek T Usmanov
{"title":"Determination of kinetic characteristics of thermal desorption of cocaine by mass-spectrometric method of surface ionization.","authors":"Ganiboy T Rakhmanov, Tursunali S Kholikov, Azim Sh Radjabov, Saida S Iskhakova, Dilshadbek T Usmanov","doi":"10.1177/14690667251358340","DOIUrl":"https://doi.org/10.1177/14690667251358340","url":null,"abstract":"<p><p>The adsorption and surface ionization of cocaine molecules C<sub>17</sub>H<sub>21</sub>NO<sub>4</sub> (<i>M</i>: 303 Da) on the surface of oxidized tungsten was studied using the non-stationary voltage modulation method in a high-vacuum mass spectrometric setup employing a \"black chamber,\" all the walls of which are cooled with liquid nitrogen. The activation energy <b>Е<sup>+</sup></b> and <b>Е<sup>0</sup></b> of thermal desorption were determined, as well as pre-exponential factors in the continuity equation for the radicals C<sub>12</sub>H<sub>8</sub>ON<i><sup>+</sup></i> and C<sub>12</sub>H<sub>8</sub>ON (<i>m/z</i> 182) during the dissociation of cocaine molecules with a break (<i>C-C</i><sub>1</sub>)<i><sub>β</sub></i> bonds with the formation of desorbing radicals by surface ionization on the surface of oxidized tungsten W<sub>x</sub>O<sub>y</sub>. The results of determining the coefficient of surface ionization, the heat of sublimation, and assessing the ionization potentials of these radicals are presented, and also determined from thermal desorption spectra of the activation energy of thermal desorption of the resulting ions in the air atmosphere.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"14690667251358340"},"PeriodicalIF":0.0,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144610946","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Mass spectrometric analysis of fullerenes and dialane cationic clusters: Revealing magic sizes and stability trends. 富勒烯和二烷阳离子团簇的质谱分析:揭示神奇的大小和稳定性趋势。
European journal of mass spectrometry (Chichester, England) Pub Date : 2025-07-10 DOI: 10.1177/14690667251358149
Namra Sarosh, Bilal Rasul
{"title":"Mass spectrometric analysis of fullerenes and dialane cationic clusters: Revealing magic sizes and stability trends.","authors":"Namra Sarosh, Bilal Rasul","doi":"10.1177/14690667251358149","DOIUrl":"https://doi.org/10.1177/14690667251358149","url":null,"abstract":"<p><p>The stability of gas-phase clusters primarily depends on their size, with magic numbers exhibiting exceptional conformal stability due to symmetric or closed-shell configurations. This phase is ideal for analyzing intrinsic properties, that is, as cluster size increases, their behavior transitions from molecular to bulk-like. The characterization of these clusters has been facilitated by advancements in mass spectrometry, which has also played a crucial role in revealing the existence of magic numbers. In this study, helium nanodroplets-doped fullerenes C<sub>60</sub> are electron-impact ionized along with dialane Al2H6 using high-resolution mass spectrometry to analyze various abundance distributions, revealing significant local irregularities (anomalies). Mass spectra of dialane-tagged C<sub>60</sub><sup>+</sup>, that is, [C<sub>60</sub>]<i><sub>m</sub></i>[Al<sub>2</sub>H<sub>6</sub>]<i><sub>n</sub></i><sup>+</sup>, display anomalies at <i>n</i> = 4 and <i>n</i> = 8 across nearly all C<sub>60</sub> cluster sizes, indicating localized irregularities. Peaks other than these magic numbers exhibit antimagic behavior. These results highlight specific mass-to-charge ratios in cationic clusters, advancing our comprehension of these complex molecules and their potential applications in nanotechnology and chemistry.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"14690667251358149"},"PeriodicalIF":0.0,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144602786","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Delivery of micro- and nanoparticles from solutions into a linear quadrupole trap using the paper spray method. 用纸喷雾法将微粒子和纳米粒子从溶液中输送到线性四极阱中。
European journal of mass spectrometry (Chichester, England) Pub Date : 2025-06-12 DOI: 10.1177/14690667251350268
M S Semynin, S S Rudyi, A Y Dubavik, A V Gavenchuk, A V Ivanov, D P Shcherbinin
{"title":"Delivery of micro- and nanoparticles from solutions into a linear quadrupole trap using the paper spray method.","authors":"M S Semynin, S S Rudyi, A Y Dubavik, A V Gavenchuk, A V Ivanov, D P Shcherbinin","doi":"10.1177/14690667251350268","DOIUrl":"https://doi.org/10.1177/14690667251350268","url":null,"abstract":"<p><p>In this paper, we develop and describe a technology for delivering micro- and nanoparticles from solutions into a linear quadrupole Paul trap using the paper spray method. The developed technology is based on electrospraying of colloids with the particles from paper cartridges into the electrodynamic trap. The proposed method has been experimentally verified using a colloid solution of AgInS<sub>2</sub>/ZnS quantum dots in toluene. It has been shown that electrospraying of the solution from a paper cartridge is observed when applying a DC voltage in the range of 5-12 kV. Stable retention of the delivered particles in the trap is observed when applying an AC voltage with a frequency of 500 Hz and an amplitude of 1000 V on the power trap electrodes and DC voltage 60-290 V on the end-cap electrode. The features of the developed technology are described in detail.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"14690667251350268"},"PeriodicalIF":0.0,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144278071","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Gas chromatography-mass spectrometry bioactive compounds profiling, potential of microbial resistance, anti-inflammatory, and cytotoxic of leaf extracts from Celtis tetrandra Roxb. 气相色谱-质谱法分析芫荽叶提取物的生物活性化合物、微生物耐药、抗炎和细胞毒性。
European journal of mass spectrometry (Chichester, England) Pub Date : 2025-06-03 DOI: 10.1177/14690667251346782
Ayesha Arshad, Shagufta Saeed, Muhammad Tayyab, Quratulain Maqsood, Tahir Mehmood
{"title":"Gas chromatography-mass spectrometry bioactive compounds profiling, potential of microbial resistance, anti-inflammatory, and cytotoxic of leaf extracts from <i>Celtis tetrandra</i> Roxb.","authors":"Ayesha Arshad, Shagufta Saeed, Muhammad Tayyab, Quratulain Maqsood, Tahir Mehmood","doi":"10.1177/14690667251346782","DOIUrl":"https://doi.org/10.1177/14690667251346782","url":null,"abstract":"<p><p>The rapid increase in incidences of antibiotic resistance, as well as the severity of side effects associated with the synthetic drugs, have directed the researchers to focus on the natural reservoirs as an alternative to the available drugs. The aim of this study was to evaluate the antimicrobial, anti-inflammatory, cytotoxicity assay, and gas chromatography-mass spectrometry (GC-MS) profiling potential of <i>C. tetrandra</i> leaf extracts. Aqueous and ethanolic extract of the leaf was prepared by the maceration process. The anti-microbial potential by disc diffusion method was estimated against <i>B. subtilis</i>, <i>S. aureus</i>, <i>E. coli</i>, and <i>S. typhi.</i> Ethanolic extract was more effective with the zone of inhibition of 18.32 ± 0.012 mm and 12.97 ± 0.02 mm against <i>S. aureus</i> and <i>E. coli</i>, respectively. Aqueous extract did not show any results against <i>S. typhi</i> and <i>B. subtilis</i>. Cytotoxicity assay on Vero cells assured the safety of the extract with IC<sub>50</sub> 920.45 μg/mL. In vivo anti-inflammatory potential was evaluated by the carrageenan-induced rat paw edema. Edema size was measured by digital Vernier caliper. The maximum paw inhibition (40.4%) was observed in the group treated with 500 mg/kg of ethanolic extract. There was a significant decrease in the level of inflammatory biomarkers such as C-reactive protein and interleukin-6, and hematological parameters. GC-MS of ethanolic extract identified the six major bioactive compound classes, including phytol, aliphatic alcohol, flavonol, sterols, and triterpenes.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"14690667251346782"},"PeriodicalIF":0.0,"publicationDate":"2025-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144210633","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Mass-spectrometric studies of kinetic characteristics of codeine molecule thermodesorption by non-stationary surface ionization method. 非固定表面电离法对可待因分子热解吸动力学特性的质谱研究。
IF 1.3
European journal of mass spectrometry (Chichester, England) Pub Date : 2022-10-01 Epub Date: 2022-11-01 DOI: 10.1177/14690667221136069
G T Rakhmanov, D T Usmanov
{"title":"Mass-spectrometric studies of kinetic characteristics of codeine molecule thermodesorption by non-stationary surface ionization method.","authors":"G T Rakhmanov,&nbsp;D T Usmanov","doi":"10.1177/14690667221136069","DOIUrl":"https://doi.org/10.1177/14690667221136069","url":null,"abstract":"<p><p>The adsorption and surface ionization of codeine molecules С<sub>18</sub>H<sub>21</sub>O<sub>3</sub>N (<i>m/z</i> 299) on the surface of oxidized tungsten have been studied by a non-stationary method of voltage modulation under the same experimental conditions with a high-vacuum mass-spectrometric setup using a \"black chamber\" all walls of which are cooled with liquid nitrogen. For the codeine molecule dissociation with the <math><mo>(</mo><mrow><mrow><mi>C</mi></mrow><mo>-</mo><msub><mrow><mi>C</mi></mrow><mn>1</mn></msub></mrow><msub><mo>)</mo><mrow><mi>β</mi></mrow></msub></math> bond breaking and formation of ionizable radicals, the rate constants <i>K</i><sup>+</sup> and <i>K</i><sup>0</sup>, the activation energy <i>Е</i><sup>+</sup> and <i>Е</i><sup>0</sup> of thermodesorption, and the pre-exponential factors in the continuity equation for the radicals C<sub>9</sub>H<sub>7</sub>N<sup>+</sup>CH<sub>3</sub> (<i>m/z</i> 144) have been defined by surface ionization on the surface of oxidized tungsten <i>W<sub>x</sub>O<sub>y</sub></i>. The results of determining the surface ionization coefficient and estimates of the ionization potentials of these radicals have been presented.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"127-131"},"PeriodicalIF":1.3,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40460477","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Bioanalytical method for estimation of procyclidine in human plasma using liquid chromatography-tandem mass spectrometry: Application to pharmacokinetic study. 液相色谱-串联质谱法测定人血浆中procylidine的生物分析方法:在药代动力学研究中的应用。
IF 1.3
European journal of mass spectrometry (Chichester, England) Pub Date : 2022-06-01 Epub Date: 2022-07-03 DOI: 10.1177/14690667221111153
Viritha Bezawada, Padma Mogili, Sireesha Dodda, Ramakrishna Gajula
{"title":"Bioanalytical method for estimation of procyclidine in human plasma using liquid chromatography-tandem mass spectrometry: Application to pharmacokinetic study.","authors":"Viritha Bezawada,&nbsp;Padma Mogili,&nbsp;Sireesha Dodda,&nbsp;Ramakrishna Gajula","doi":"10.1177/14690667221111153","DOIUrl":"https://doi.org/10.1177/14690667221111153","url":null,"abstract":"<p><p>A rapid, selective and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for quantification of procyclidine hydrochloride in human plasma using Procyclidine D11 hydrochloride as internal standard. Liquid-liquid extraction technique with methyl tertiary butyl ether was used for the extraction of plasma samples. Chromatographic separation of the analyte and the internal standard from the endogenous components was done on Zodiac C<sub>18</sub> column (50 × 4.6 mm, 5 µm) using a mixture of methanol and 0.1% formic acid in water (70:30, v/v) as mobile phase at a flow rate of 1 mL/min with the run time of 2 min. The detection of the eluents was done using multiple reaction monitoring (MRM) in positive ion mode. Linearity of the method was established in the concentration range of 0.5 to 120 ng/mL. Full validation of the method was done as per USFDA guidelines and the results were well within the acceptance limits. The successful application of the method was done on healthy human subjects under fasting conditions, proving it to be used for bioequivalence and bioavailability (BA/BE) studies of procyclidine.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"89-93"},"PeriodicalIF":1.3,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40470264","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Differential ionization cross-section of hydrogen bromide. 溴化氢的微分电离截面。
IF 1.3
European journal of mass spectrometry (Chichester, England) Pub Date : 2022-06-01 Epub Date: 2022-09-28 DOI: 10.1177/14690667221129942
Ritu Sharawat, Meenakshi Kumari, Rajeev Kumar, Ravinder Sharma
{"title":"Differential ionization cross-section of hydrogen bromide.","authors":"Ritu Sharawat,&nbsp;Meenakshi Kumari,&nbsp;Rajeev Kumar,&nbsp;Ravinder Sharma","doi":"10.1177/14690667221129942","DOIUrl":"https://doi.org/10.1177/14690667221129942","url":null,"abstract":"<p><p>In this study, the relative single and double differential ionization cross-section of the hydrogen bromide molecule and their fragmented ions (HBr<sup>+</sup>, Br<sup>+</sup>, H<sup>+</sup>) have been theoretically evaluated. In the single differential ionization cross-sections, the loss of incident electron energies (W) at 100 eV, 200 eV, and 500 eV is calculated. The double differential ionization cross-section of the HBr molecule is determined for secondary electron energy (e) and different incident scattering angles (θ). The differential ionization cross-sections of the hydrogen bromide molecule were investigated for the first time.The derived results of the HBr molecule are not only important in spectrometry but may also be interesting for atmospheric sciences.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"75-80"},"PeriodicalIF":1.3,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40379256","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application. 一种简单的核壳柱超高效液相色谱-质谱联用法测定人血浆中依西美坦的临床应用。
IF 1.3
European journal of mass spectrometry (Chichester, England) Pub Date : 2022-06-01 Epub Date: 2022-09-21 DOI: 10.1177/14690667221126276
Takuho Ishii, Nana Nojiri, Yuji Mano
{"title":"A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application.","authors":"Takuho Ishii,&nbsp;Nana Nojiri,&nbsp;Yuji Mano","doi":"10.1177/14690667221126276","DOIUrl":"https://doi.org/10.1177/14690667221126276","url":null,"abstract":"<p><p>Exemestane is one of the aromatase inhibitors and has been used to treat breast cancer by lowering estrogen levels. Accurate quantification of exemestane is important to set an optimal dose, and thus a simple assay for exemestane is developed by ultra-performance liquid chromatography with tandem mass spectrometer. Exemestane was extracted from human plasma samples (100 μL) by simple protein precipitation with acetonitrile/methanol (1/1, v/v). Interference peaks observed close to the elution of exemestane led us to use a core shell column for higher selectivity instead of totally porous columns. The extracts were chromatographed on CORTECS UPLC C18, under a gradient elution at a flow rate of 0.25 mL/min and detected in the selected reaction monitoring. Validation parameters were assessed in accordance with the bioanalytical guidelines using quality control samples. Exemestane in human plasma was quantifiable from 0.5 to 50 ng/mL with high extraction recovery and minimal matrix effects. Hemolyzed or hyperlipemic plasma did not impact the exemestane assay. Exemestane was stable in human plasma for 392 days at -15°C or below. The developed assay was robust and successfully applied to quantifying exemestane concentrations in human plasma to support a clinical trial.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"94-103"},"PeriodicalIF":1.3,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40373079","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Gas chromatography-mass spectrometric determination of organic acids by ion pair liquid extraction followed by in-situ butylation from aqua feed samples. 气相色谱-质谱联用离子对液体萃取-原位丁化法测定水产饲料样品中的有机酸。
IF 1.3
European journal of mass spectrometry (Chichester, England) Pub Date : 2022-02-01 Epub Date: 2022-06-23 DOI: 10.1177/14690667221103227
Kalpana Talari, Sai Krishna Ganji, Satish Mutyam, Raja Rajeswari Tiruveedula
{"title":"Gas chromatography-mass spectrometric determination of organic acids by ion pair liquid extraction followed by in-situ butylation from aqua feed samples.","authors":"Kalpana Talari,&nbsp;Sai Krishna Ganji,&nbsp;Satish Mutyam,&nbsp;Raja Rajeswari Tiruveedula","doi":"10.1177/14690667221103227","DOIUrl":"https://doi.org/10.1177/14690667221103227","url":null,"abstract":"<p><p>A rapid and sensitive analytical method was developed to quantitatively determine organic acids (OAs) from fish feed samples extracted by ion-pair (IP) solvent extraction, followed by in-situ butylation and gas chromatography-mass spectrometric (GC-MS) analysis. The extraction of OAs was carried out with acetonitrile containing 10 mM tetrabutylammonium hydroxide (TBAH), and the analytes were derivatized to their butyl esters in the injection port of the GC-MS system. The developed method was validated in the range of 1-5000 ng/g, with recoveries ranging from 93-117%. The limit of detection (LOD) and limit of quantification (LOQ) of the method was 1-5 ng/g and 2-10 ng/g, respectively, yielding good linearity (R<sup>2</sup> > 0.9990) and precision with a relative standard deviation less than 10%. The proposed method was successfully applied to analyze OAs in sinking and floating fish feed samples. The analyzed samples showed the presence of benzoic, succinic, fumaric, glutaric, adipic, and phthalic acids in sinking feed samples; and benzoic, succinic, adipic, phthalic acids in floating feed samples, respectively.</p>","PeriodicalId":520618,"journal":{"name":"European journal of mass spectrometry (Chichester, England)","volume":" ","pages":"25-34"},"PeriodicalIF":1.3,"publicationDate":"2022-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40391241","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 1
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