• Mass Spectrometry Letters
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• 제4권3호
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• pp.55-58
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• 2013

Dioscin is a biologically active steroidal saponin with anticancer and hepatoprotective effects. A rapid, selective, and sensitive liquid chromatographic method with electrospray ionization tandem mass spectrometry was developed for the quantification of dioscin in rat plasma. Dioscin was extracted from rat plasma using ethyl acetate at acidic pH. The analytes were separated on a Halo C18 column using gradient elution of acetonitrile and 0.1% formic acid and detected by tandem mass spectrometry in selected reaction monitoring mode. The standard curve was linear ($r^2$ = 0.998) over the concentration range of 1-100 ng/mL. The lower limit of quantification was 1.0 ng/mL using 50 ${\mu}L$ of plasma sample. The coefficient of variation and relative error for intra- and inter-assay at four QC levels were 1.3 to 8.0% and -5.4 to 10.0%, respectively. This method was applied successfully to the pharmacokinetic study of dioscin after oral administration of dioscin at a dose of 29.2 mg/kg in male Sprague-Dawley rats.

• 분석과학
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• 제36권2호
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• pp.89-98
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• 2023

Analytical methods for detecting atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes were developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). UHPLC-MS/MS conditions were optimized for rapid, sensitive, and simultaneous analysis of the five allergenic compounds. The methods were validated by assessing their specificity, matrix effects, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and precision. Good linearity was achieved with a determination coefficient of ≥0.99. The LOD and LOQ were 2.1-9.8 and 6.4-29.6 ng/g for sanitary napkins and 0.29-0.48 and 0.87-1.45 ng/mL for mouthwashes, respectively. The accuracy and precision were within an acceptable range according to the criteria reported in the European SANTE/11813/2017 guidelines (70-120 % recovery, <20 % relative standard deviation). Therefore, these methods can be used to analyze atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes.

• 분석과학
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• 제37권5호
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• pp.271-279
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• 2024

Bisphenols and phthalates are endocrine-disrupting chemicals that are commonly used in packaging and as plasticizers. However, they pose health risks through ingestion, inhalation, and dermal contact. Accurate analysis of these pollutants is challenging owing to their low concentration and their presence in complex oil matrices. Therefore, they require efficient extraction and detection methods. In this study, an analytical method for the simultaneous quantification of bisphenols and phthalates in corn oil is developed. The dynamic multiple reaction monitoring mode of liquid chromatography-tandem mass spectrometry is used according to the different polarities of bisphenols and phthalates. The method is validated by assessing system suitability, linearity, accuracy, precision, homogeneity, and stability. The determination coefficients are higher than 0.99, which is acceptable. The percentage recovery and coefficient of variation of the accuracy and precision confirm that this analytical method is capable of simultaneously quantifying bisphenols and phthalates in corn oil. The bisphenols and phthalates in the formulations and pretreatment samples are stable for 7 d at room temperature and 24 h in an auto-sampler. Therefore, this validated analytical method is effective for the simultaneous quantification of bisphenols and phthalates in oils.

• Mass Spectrometry Letters
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• 제5권2호
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• pp.52-56
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• 2014

Glycated hemoglobin (HbA1c) is used as an index of mean glycemia over prolonged periods. This study describes an optimization of enzyme digestion conditions for quantification of non-glycated hemoglobin (HbA0) and HbA1c as diagnostic markers of diabetes mellitus. Both HbA0 and HbA1c were quantitatively determined followed by enzyme digestion using isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) with synthesized N-terminal hexapeptides as standards and synthesized isotope labeled hexapeptides as internal standards. Prior to quantification, each peptide was additionally quantified by amino acid composition analysis using ID-LC-MS/MS via acid hydrolysis. Each parameter was considered strictly as a means to improve digestion efficiency and repeatability. Digestion of hemoglobin was optimized when using 100 mM ammonium acetate (pH 4.2) and a Glu-C-to-HbA1c ratio of 1:50 at $37^{\circ}C$ for 20 h. Quantification was satisfactorily reproducible with a 2.6% relative standard deviation. These conditions were recommended for a primary reference method of HbA1c quantification and for the certification of HbA1c reference material.

• Mass Spectrometry Letters
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• 제11권3호
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• pp.59-64
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• 2020

Mertansine, a thiol-containing maytansinoid, is a tubulin inhibitor used as the cytotoxic component of antibody-drug conjugates for the treatment of cancer. Liquid chromatography-tandem mass spectrometry was described for the determination of mertansine in rat plasma. 50-μL rat plasma sample was pretreated with 25 μL of 20 mM tris-(2-carboxyethyl)-phosphine, a reducing reagent, and further vortex-mixing with 50 μL of 50 mM N-ethylmaleimide for 3 min resulted in the alkylation of thiol group in mertansine. Alkylation reaction was stopped by addition of 100 μL of sildenafil in acetonitrile (200 ng/mL), and following centrifugation, aliquot of the supernatant was analyzed by the selected reaction monitoring mode. The standard curve was linear over the range of 1-1000 ng/mL in rat plasma with the lower limit of quantification level at 1 ng/mL. The intra- and inter-day accuracies and coefficient variations for mertansine at four quality control concentrations were 96.7-113.1% and 2.6-15.0%, respectively. Using this method, the pharmacokinetics of mertansine were evaluated after intravenous administration of mertansine at doses of 0.2, 0.5, and 1 mg/kg to female Sprague Dawley rats.

• Bulletin of the Korean Chemical Society
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• 제25권1호
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• pp.109-114
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• 2004

A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

• Mass Spectrometry Letters
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• 제7권1호
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• pp.26-29
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• 2016

Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r² value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

• Mass Spectrometry Letters
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• 제2권1호
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• pp.8-11
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• 2011

Two types of glycerolipids [monoacylglycerols (MAG) and cyclitols] were isolated by reversed phase high-performance liquid chromatography from the methanol extracts of a marine sponge, and analyzed by fast atom bombardment mass spectrometry (FAB-MS) in positive-ion mode. FAB mass spectra of these compounds yielded protonated molecules $[M + H]^+$ and abundant sodiated molecules $[M + Na]^+$ from a mixture of 3-nitrobenzyl alcohol and NaI. The structures of these compounds were elucidated by FAB-collisional-induced dissociation (CID)-tandem mass spectrometry. We carried out collision-indused dissociation (CID) of these lipids in B/E-linked scan mode. The CID B/E-linked scan of $[M + H]^+$ and $[M + Na]^+$ precursor ions resulted in the formation of numerous characteristic product ions through a series of dissociative processes. The product ions formed by charge-remote fragmentation (CRF) provided important information for the identification of the acyl chain structure substituted at the glycerol backbone. Some of the product the ions were diagnostic for the presence of a glycerol backbone or acyl chain structure.

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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• pp.288.3-289
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• 2003

Sphingolipid species are important second messengers due to their role in the mitogenesis, differentiation and apoptosis. We developed a new column liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) in combination with multiple reaction monitoring (MRM) method for the rapid, simultaneous and quantitative determination of unambiguous detecting sphingolipids in cell culture of human cancer cells (HL-60). (omitted)

• 대한약학회:학술대회논문집
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• 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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• pp.401.3-402
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• 2002

Enalapril (ENP) maleate is effective drug for the treatment of renivascular hypertension and heart failure. ENP acts as inhibitor of the enzyme angiotensin-convertase (ACE-inhibitor) and metabolized to enalaprilat (ENPT), which is the active metabolite that is really responsible for the therapeutic action. In the present study, a sensitive and rapid liquid chromatography/ electrospray ion trap tandem mass spectrometry (LC/MS/MS) method combined with high-throughput solid phase extraction (SPE) has been developed and validated for the simultaneous quantitative determination of ENP and ENPT in human plasma. (omitted)