• Journal of Applied Biological Chemistry
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• 제65권1호
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• pp.17-21
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• 2022

생약 중 잔류농약의 안전성을 확보하기 위해 metalaxyl에 대해 백출과 우슬의 잔류농약 분석법을 개발하고자 하였다. LC-MS/MS를 사용하여 QuEChERS법을 기반으로 백출과 우슬 중 metalaxyl을 분석하기 위하여 물로 습윤화 시켜 acetonitirile로 추출하여 MgSO₄와 NaCl을 첨가해 층 분리 후 SPE-NH₂ cartridge로 정제하였다. 본 분석법의 기기정량한계와 분석정량 한계는 0.002 ㎍/mL과 0.01 mg/kg이었고 표준검량선은 0.001-0.05 mg/L 범위에서 결정계수(R²) 0.999의 직선성을 확인하였다. 백출과 우슬에 대한 회수율은 MLOQ 수준, MLOQ의 10배 수준에서 88.1-109.1%의 우수한 회수율을 보였고, 변이계수는 2.0-6.2%로 10%이하였다. 본 연구에서 확립한 LC-MS/MS를 이용한 잔류분석법의 회수율 및 분석오차는 국제적인 기준을 만족하고 있으므로 생약 백출 및 우슬 중 metalaxyl의 안전성 검사를 위한 분석법으로 활용할 수 있을 것이라고 판단된다.

• Bulletin of the Korean Chemical Society
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• 제35권3호
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• pp.821-827
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• 2014

An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

• Bulletin of the Korean Chemical Society
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• 제29권11호
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• pp.2125-2128
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• 2008

• 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.277.2-278
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• 2003

A liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the determination of tiropramide in human plasma was developed. Tiropramide and internal standard, cisapride were extracted from human plasma with MTBE at basic pH. A reverse-phase LC separation was performed on Luna C8 column with the mixture of acetonitrile-ammonium formate (10 mM, pH 4.5) (5:5, v/v) as mobile phase. (omitted)

• 약학회지
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• 제49권3호
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• pp.212-216
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• 2005

A rapid, sensitive and selective electrospray tandem mass spectrometric (ESI-LC/MS/MS) method for the quantitation of gliquidone in human plasma was developed. A bioavailability study of gliquidone tablet (30 mg gliquidone, Boehringer Ingelheim Korea Co.) was performed using the validated ESI-LC/MS/MS method. The dose of 30 mg of gliquidone (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 5, 7, 9, 12, 24, and 33 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $10\~1000 ng/ml$. The coefficient of variation for intra- and inter-day assay were $8.30\~18.86$, and $2.19\~12.92\%$, respectively. The lower limit of quantification for gliquidone was 10 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 3861.17$\pm$1328.61 ng-hr/ml, $C_{max}$ was 831.02$\pm$227.99 ng/ml, $T_{max}$ was $2.94{\pm}0.77 hr,\;K_e$, was 0.19$\pm$0.06 1/hr, and $t_{l/2}$ was 4.47$\pm$3.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of gliquidone dosage forms was prepared successfully and could be used for the bioequivalence test of gliquidone preparation.

• 약학회지
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• 제49권3호
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• pp.225-229
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• 2005

A rapid, sensitive and selective tandem mass spectrometric method (LC-MS/MS) for the quantitation of nicorandil in human plasma was developed. A bioavailability study of Sigmat tablet (5 mg nicorandil, Choongwae Co.) was per-formed using the validated LC-MS/MS method. The dose of 5 fig of nicorandil (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.25, 0.5, 1, 2, 3, 4, 5, 6, 9, 12, and 24 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $0.5\~200.0 ng/ml$. The coefficient of variation for intra- and inter-day assay were $3.55\~7.44$, and $2.17\~9.102\%$, respectively. The lower limit of quantification for nicorandil was 0.5 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 145.9$\pm$83.0 ng-hr/ml, Cmax was 83.8$\pm$32.2 ng/ml, $C_{max}$ was 0.42$\pm$0.13 hr, $K_e$ was 0.56$\pm$0.23 l/hr, and $t_{l/2}$ was 1.42$\pm$0.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of nicorandil dos-age forms was prepared successfully and could be used for the bioequivalence test of nicorandil preparation.

• 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.251.2-251.2
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• 2002

2-Methylaminoethyl- 4,4' -dimethoxy- 5, 5',6,6' -dimethylenedioxybiphenyl- 2' -carboxy- 2-carboxylate (DDB-S) is a synthetic compound derived from DDB. which is protects liver against carbon tetrachloride-, D-galactosamine-, thioacetamine-, and prednisolone- induced hepatic injury in experimental animals. We assessed the use of liquid chromatography/electrospray iontrap tandem mass spectrometry (LC/MS/MS) method to identify and quantify in vivo metabolites and to measure excretion. (omitted)

• 한국축산식품학회지
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• 제35권6호
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• pp.765-771
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• 2015

The development of a sample preparation method and optimization of the analytical instrumentation conditions were performed for the determination of the vitamin B₁₂ content in emulsified baby foods sold on the Korea market. After removal of the milk protein and fats by chloroform extraction and centrifugation, the vitamin B₁₂ was water extracted from the sample. Following filtration of the solution through a nylon filter, the water-soluble extract was purified by solid-phase extraction using a Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS). The solution eluted from the cartridge was dried under a stream of nitrogen gas and reconstituted with 1 mL of water. The sample solution was injected into an LC-MS/MS system after optimizing the mobile phase for vitamin B₁₂ detection. The calibration curve showed good linearity with the coefficient of correlation (r²) value of 0.9999. The limit of detection was 0.03 µg/L and the limit of quantitation was 0.1 µg/L. The method of detection limit was 0.02 µg/kg. The vitamin B₁₂ recovery from a spiking test was 99.62% for infant formula and 99.46% for cereal-based baby food. The sample preparation method developed in this study would be appropriate for the rapid determination of the vitamin B₁₂ content in infant formula and baby foods with emulsified milk characteristics. The ability to obtain stable results more quickly and efficiently would also allow governments to exercise a more extensive quality control inspection and monitoring of products expected to contain vitamin B₁₂. This method could be implemented in laboratories that require time and labor saving.

• 분석과학
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• 제31권1호
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• pp.39-46
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• 2018

온라인 고체상 추출을 이용한 LC/MS/MS를 사용하여 carbaryl과 유기인계 농약 7 종을 동시에 분석하는 방법을 확립하였다. 분석 대상농약은 carbaryl, diazinon, methyl-demeton, fenitrothion, malathion, parathion, phenthoate, EPN 등 8 종이다. 본 연구에서는 온라인 고체상 추출과 LC/MS/MS의 ESI positive mode로 전처리 없이 물 시료 $500{\mu}L$를 직접 주입하여 10분안에 분석하였다. 농약 8 종의 회수율은 86.8~100 % 였고, 정확도는 90.6~98.8 %로 90 %이상이었고, 정밀도는 1.3~5.2 %로 나타났으며 검출한계 및 정량한계는 각각 $0.05{\sim}0.28{\mu}g/L$, $0.16{\sim}0.89{\mu}g/L$ 였다. $0.5{\mu}g/L$에서 $8.0{\mu}g/L$까지 다섯 개의 농도로 검량선을 작성한 결과 모든 물질의 상관계수(r2)가 0.99이상을 나타냈다. 방법의 유효성 평가를 한 결과 모든 내용에서 적합하므로확립한 분석방법으로 수질 시료에서 농약을 조사한 결과 모두 검출되지 않았다.

• 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.