• Bulletin of the Korean Chemical Society
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• 제30권2호
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• pp.368-372
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• 2009

The trace polymer and additives in used stripper solutions were analyzed by a combination of Py-GC/MS and ESI-MS. In the comparison of the pyrolysates produced by the pyrolysis of the pure stripper and photoresist at $500{^{\circ}C}$, the presence of novolac polymer in the used stripper was confirmed by the presence of the characteristic peaks of its pyrolysates, such as those of the methylphenol, di-methylphenol and methylenebis(methylphenol) isomers. The intact trace polymer was measured by ESI-MS, which showed the distribution of oligomers at intervals of 120 Da, indicating di-methylphenol to be the repeat unit. Additional MS/MS measurements demonstrated that the end group is methylphenol and the repeat groups are di-methylphenol. Some modified oligomers caused by the methylation or di-methylation of the repeat unit were also identified. Although the polymer is only present at a trace level in the used stripper, these combined analytical methods provided the means to qualify the stripper solution through the identification and structural determination of the polymer.

• 약학회지
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• 제51권2호
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• pp.96-102
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• 2007

Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in urine has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. A simple, rapid, and highly sensitive analytical method for Gb3 in urine was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Only simple 5-fold dilution of urine is necessary for the extraction and isolation of Gb3 in urine. Gb3 in diluted urine was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Eight isoforms of Gb3 were completely resolved from urine matrix. C24:0 Gb3 occupied 50% of total Gb3 as a major component in urine. Linear relationship for Gb3 isoforms was found in the range of 0.005${\sim}$5.0 ${\mu}$g/ml. The limit of detection (S/N=5) was 0.005 ${\mu}$g/ml and limit of quantification was 0.05 ${\mu}$g/ml for C24:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9598 to 0.9975. This method could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

• 분석과학
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• 제22권4호
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• pp.326-335
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• 2009

계란 중에 잔류하는 6 종의 글루코코티코이드 약물을 극미량으로 분석하는 방법이 개발되었다. 동시분석을 위한 시료 추출방법과 정제방법을 확립하였으며 액체 크로마토그래프와 질량분석기의 최적화 조건을 확립하였으며, 글루코코티코이드를 분석하기 위해서는 5 g의 계란에 초산 완충용액을 사용하여 시료의 pH를 5.2로 조절한 후 효소 가수분해를 위해 Helilx pomatia를 사용하였다. 혼합물을 원심분리하여 20 mL n-헥산으로 두 번 추출하였다. 다시 HLB 카트리지에서 메탄올에 의한 추출이 이루어진 후 연속해서 실리카 카트리지에서 메탄올/에틸아세테이트를 사용하여 정제하였다. 분석물질은 역상 HPLC/ESI-MS/MS로 분석하였으며 ESI는 음이온 모드를 사용하였다. 검정곡선의 상관계수는 0.99 이상을 나타내었고 검출한계는 $0.09-0.17{\mu}g/kg$ 이었으며 회수율은 55.7-69.8%이었다. 바탕 계란 중에서 실험된 유효성 검증방법에 근거하여 확립된 분석법은 계란 중 글루코코티코이드를 수 ${\mu}g/kg$ 농도까지 검출하는데 사용될 수 있을 것이다.

• Mass Spectrometry Letters
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• 제3권3호
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• pp.68-73
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• 2012

Fat malabsorption is an important cause of poor growth in infancy and childhood. Steatorrhea tests have been developed using various methods. Traditional measurements of stool fat, however, require large samples and it often takes as a week to complete the analysis. In this paper, a liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI/MS) method was developed for simultaneous quantitative analysis of triacylglycerols, triolein, diolein and monoolein, in mouse feces. Moreover, the procedure was rapid, simple as well as compatible with LC-ESI/MS. Chloroform-isopropyl alcohol solution was used for fat-soluble sample extraction. After centrifugation and filtration, an analytical solution was prepared. Triolein, diolein and monoolein were separated using non-aqueous reversed-phase column with the mobile phase consisting of A (methanol) and B (acetone-isopropyl alcohol). The precision (% CV) and accuracy (% bias) of the assay were 3.8-14.7% and 85.2-114.9%, respectively. This method has been successfully applied to simultaneous determination of triolein, diolein and monoolein in feces from 30 mice. This method can therefore be applied to measure triacylglycerols in mouse feces accurately and precisely by LC-ESI/MS, thereby helping to predictive biomarker in fat malabsorption and diagnostic research.

• 생약학회지
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• 제43권2호
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• pp.137-146
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• 2012

Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.

• 생약학회지
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• 제44권4호
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• pp.350-361
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• 2013

Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

• Mass Spectrometry Letters
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• 제8권2호
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• pp.29-33
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• 2017

Understanding the mechanisms that control and concentrate the observed electrospray ionisation (ESI) response from peptides is important. Controlling these mechanisms can improve signal-to-noise ratio in the mass spectrum, and enhances the generation of intact ions, and thus, improves the detection of peptides when analysing mixtures. The effects of different mixtures of aqueous: organic solvents (25, 50, 75%; v/v): formic acid solution (at pH 3.26) compositions on the ESI response and charge-state distribution (CSD) during mass spectrometry (MS) were determined in a group of biologically active peptides (molecular wt range 1.3 - 3.3 kDa). The ESI response is dependent on type of organic solvent in the mobile phase mixture and therefore, solvent choice affects optimal ion intensities. As expected, intact peptide ions gave a more intense ESI signal in polar protic solvent mixtures than in the low polarity solvent. However, for four out of the five analysed peptides, neither the ESI response nor the CSD were affected by the volatility of the solvent mixture. Therefore, in solvent mixtures, as the composition changes during the evaporation processes, the $pK_b$ of the amino acid composition is a better predictor of multiple charging of the peptides.

• Mass Spectrometry Letters
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• 제4권4호
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• pp.83-86
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• 2013

A new interface for coupling CIEF and MS using a four-way cross has been developed in a single mechanical system. This new interface could be operated without the electric discontinuity and reinstallation of lines. Additionally, a bare fused silica capillary was facilitated as a spray needle to produce electrospray and to guide catholyte or sheath liquid. Focusing for CIEF was completed in a hanging droplet at the end of spray needle. This capillary spray needle also provided stable spray, enhanced the ionization efficiency and increased sensitivity. Results with carbonic anhydrase I showed that focusing and spraying were well completed with the new interface and the new spray needle.

• 한국응용과학기술학회지
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• 제33권2호
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• pp.255-263
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• 2016

식품부패미생물에 대한 감초추출물의 항균력을 확인하고 유효성분을 분리한 후 그 구조를 확인 하였다. 감초추출물은 대표적인 항균제인 메타중아황산칼륨과 myconazole과 비슷한 항균 활성을 나타내었다. 용매분획을 실시한 결과 chloroform fraction이 가장 항균활성이 높은 것으로 나타났다. 이에 chloroform분획을 silica gel column chromatography를 통해 분리하여 항균활성이 가장 큰 분획물인 KC를 분리하였다. 이 화합물은 ESI-MS 와 $^1H$-NMR, $^{13}C$-NMR 결과로부터 활성물질의 구조를 동정하였으며 그 결과 KC는 (R)-glabridin인 것으로 확인하였다.

• 한국자원식물학회지
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• 제30권6호
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• pp.693-698
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• 2017

The quality control of natural products is principal key to guarantee the Good Manufacturing Practices (GMP) and Good Clinical Practices (GCP) for the functional food, pharmaceuticals and cosmeceuticals in the industry. In this study, we examined the quantitative analysis of berberine as marker substance of Coptidis Rhizoma by high performance liquid chromatography-photodiode array detector (HPLC-DAD). The HPLC method was validated and met all the requirements for the quality control analysis recommended by FDA and ICH. The berberine was separated on a Xterra $C_{18}$ column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of distilled water and acetonitrile with $KH_2PO_4$ (3.4 g) and $Na_2SO_4$ (1.7 g). Calibration curve of berberine has been estimated (y = 42293.47x-41589 with the correlation coefficient 0.9999). The amount of berberine was calculated as 4.25%. And berberastine, palmatine, columbamine, jatrorrhizine, epiberberine, berberine and coptisine in the Coptidis Rhizoma were identified by high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-ESI-MS) method.