• 분석과학
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• 제23권4호
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• pp.405-413
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• 2010

축산물(소의 근육 및 간)중에 잔류하는 합성 글루코코티코이드 6종 (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, flumethasone)에 대한 동시분석방법을 확립하였다. 효과적인 기기분석을 위해서 시료는 C18 고체상 카트리지를 사용하여 에틸아세테이트 용매를 사용하여 추출/정제하였다. C18 컬럼을 사용하여 분리한 후 음이온 전기분무 질량분석법의 multiple reaction monitoring 방법을 사용하여 정량 및 정성 분석을 수행하였다. 효과적이고 감도있는 HPLC-MS/MS 분석을 위해서 0.1% 포름산이 포함된 물과 아세토나이트릴이 이동상 용매로 사용되었다. 메트릭스와 약물의 종류에 따라서 검출한계(LOD)는 $0.2-0.1\;{\mu}g$/kg, 정량한계(LOQ)는 $0.8-3.4{\mu}g$/kg 이었으며, 회수율은 89.5-119.6%이었다. 확립된 기존의 방법들에 비해 6종의 글루코코티코이드의 동시분석 방법이 간소화되었고, 좋은 정확도, 정밀도 및 회수율을 나타내었으며, 축산 육류 중에 잔류하는 글루코코티코이드들 분석하는데 사용될 수 있을 것이다.

• 약학회지
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• 제60권2호
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• pp.64-72
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• 2016

Jakyakgamcho-tang is a well-known traditional herbal medicine and has been used for the treatment of mainly pains in oriental medicine. In this study, analytical method for the quantitative determination of the eleven marker components, gallic acid (1), oxypaeoniflorin (2), paeoniflorin (3), albiflorin (4), liquiritin (5), isoliquiritin (6), ononin (7), liquiritigenin (8), benzoylpaeoniflorin (9), paeonol (10), and glycyrrhizin (11) in Jakyakgamcho-tang decoction was performed using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer. The analytical column for separation of the compounds 1~11 was used an UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$) column and column oven temperature was maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid (A) and acetonitrile (B) by gradient elution. The flow rate was 0.3 ml/min and injection volume was $2.0{\mu}l$. Correlation coefficient in the calibration curves of the compounds 1~11 were showed a good linearity with more than 0.99. The limit of detection and limit of quantification values of the compounds 1~13 were detected in the ranges 0.06~18.43 ng/ml and 0.18~58.29 ng/ml, respectively. Among the compounds 1~11, the compounds 10 were not detected in this sample, while the ten compounds, 1~9 and 11, were detected $44.05{\sim}19,289.05{\mu}g/g$ in Jakyakgamcho-tang extract.

• 한국동물위생학회지
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• 제25권1호
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• pp.23-29
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• 2002

A method was developed to separate, detect and qualify aldicarb, bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur in meats and fruits. Experimental beef and fork samples were fortified with 0.05mg/kg of carbamate pesticides for analysis. Carbamate-detected pear by HPLC fluorescence detector(HPLC/FLS) are extracted with acetonitril and refined by solid phase extraction(SPE) filled with aminopropyl-bonded silca, In the following step, the injected materials into LC/MS are analyzed to result in the fact that bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur presents several sorts of fraction ions following with; [M+H]$^{+}$, [M+Na]$^{+}$,［M-CONH$CH_3$]$^{+}$, [M-OCONH$CH_3$]$^{+}$. In addition, ethiofencarb presents [M-SCH$_2$$CH_3$]$^{+}$ ion distinctive and aldicarb presents [M+Na]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ ion which is the most decisive fraction ion for pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur excluding [M+H]$^{+}$ ion. However, [M-OCONH$CH_3$]$^{+}$ and [M-OCONH$CH_3$]$^{+}$ fraction ion charactering carbamate pesticides are detected most efficiently with fragment voltage 50ev. As a result, for rluantitative analysis, [M+Na]$^{+}$ ion is the most decisive ion for detection of aldicarb and [M+H]$^{+}$ ion is the most decisive fraction ion for Pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur. Carbaryl-detected pear by HPLC/FLS are analyzed by L/MS and the result shows that [M+H]$^{+}$ and [M-CONH$CH_3$]$^{+}$ ions charactering carbaryl are detected.ering carbaryl are detected.

• 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.

• 한국식품과학회지
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• 제44권4호
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• pp.390-392
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• 2012

LC/MS/MS로 패류 114건에서 설사성패독인 OA, DTX1, PTX2, YTX을 정량한 결과 110건(96.5%)에서는 설사성패독이 불검출이었으며, 굴 2건(0.004, 0.001 ${\mu}g/g$), 진주담치 1건(0.001 ${\mu}g/g$), 바지락 1건(0.001 ${\mu}g/g$)에서 OA(Okadaic acid)가 검출되어 3.5%의 검 출률을 나타내었으며 동일 시료를 마우스시험법으로 마비성 패독을 실험한 결과 설사성 패독과의 유의성은 보이지 않았다.

• Natural Product Sciences
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• 제22권2호
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• pp.93-101
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• 2016

For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH $C_{18}$ column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ${\geq}0.9920$ within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and $115.01{\mu}g/g$, respectively.

• 생약학회지
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• 제43권1호
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• pp.10-15
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• 2012

An accurate and sensitive analysis method was established for simultaneous determination of three bioactive compounds (glycyrrhizin, 6-gingerol and ginsenoside Rg3) in the Ejung Tang with high-performance liquid chromatography (HPLC)-photodiode array detection (DAD)-electrospray ionization (ESI)-Mass spectrometry (MS). The optimizing chromatographic separations a were acquired by an $C_{18}$ column ($5{\mu}m$, $4.6I.D{\times}250mm$, SHISHEDO) using gradient elution with water comprising 0.1% TFA(trifluoroacetic acid) and acetonitrile at a performing temperature of $35^{\circ}C$. Flow rate was 1.0 ml/min. A detection UV wavelength set at 205 nm and 250 nm. The three compounds were identified by electrospray ionization mass spectrometry. All calibration curves indicated great linear regression within test ranges ($R^2>0.9997$). The established method provided acceptable precision and accuracy. The relative standard deviations (RSDs) of intra-day and inter-day were less than 2.00% and 3.00%, respectively. The recoveries were found to range from 94.49 to 101.10% for the three compounds analyzed. These results showed that this method was effective and reliable for quality control of Eiung-Tang.

• Mass Spectrometry Letters
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• 제12권4호
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• pp.179-185
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• 2021

Collision-induced dissociation (CID) combined with electrospray ionization mass spectrometry (ESI-MS) was used to obtain structural information on rat islet amyloid polypeptide (rIAPP) monomers (M) and dimers (D) observed in the multiply charged state in the MS spectrum. MS/MS analysis indicated that the rIAPP monomers adopt distinct structures depending on the molecular ion charge state. Peptide bond dissociation between L₂₇ and P₂₈ was observed in the MS/MS spectra of rIAPP monomers, regardless of the monomer molecular ion charge state. MS/MS analysis of the dimers indicated that D⁵⁺ comprised M²⁺ and M³⁺ subunits, and that the peptide bond dissociation process between the L₂₇ and P₂₈ residues of the monomer subunit was also maintained. The observation of (M+ b₂₇)⁴⁺ and (M+ y₁₀)³⁺ fragment ions were deduced to originate from the two different D⁵⁺ complex geometries, the N-terminal and C-terminal interaction geometries, respectively. The fragmentation pattern of the [M_rIAPP + M_hIAPP]⁵⁺ MS/MS spectrum showed that the interaction occurred between the two N-terminal regions of M_rIAPP and M_hIAPP in the heterogeneous dimer (hetero-dimer) D⁵⁺ structure.

• 융합정보논문지
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• 제11권2호
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• pp.107-116
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• 2021

본 연구에서는 동물식품 내 잔류하는 동물의약품 중 성장보조제인 에스트라디올(Estradiol-17��), 테스토스테론(Testosterone), 프로게스테론(Progesterone)에 대한 분석법을 개발하고자 하였다. 분석대상 물질은 액체크로마토그라피를 사용하여 분리하였고, electrospray ionization(ESI) 과정을 거쳐 질량분석기에 주입되어 multiple reaction monitoring(MRM) 모드로 검출하였다. 개발된 분석법은 CODEX CAC/GL 71-2009에 근거하여 유효성을 검증하였고, 분석의 실효성 허용범위를 충족함을 확인하였다. 국내 유통되는 소고기, 돼지고기, 닭고기에 대해 확립된 분석법으로 분석을 진행하여 실제시료 적용성을 확인하였다. 이를 통해 개발된 분석법이 국내 유통 축산물에서 확인되고 있는 성장보조제 일부에 대해 신속하고 신뢰성 높은 분석이 가능함을 확인하였다. 후속 연구를 통해 확립된 분석법을 기반으로 분석대상 성장보조제의 범위를 확장하고, 이를 모두 포함시켜 동시분석법을 확립한다면 활용성이 높은 분석법이 완성될 것으로 확신한다.

• Mass Spectrometry Letters
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• 제13권4호
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• pp.177-183
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• 2022

The monomer and dimer structures of the amyloid fragment Aβ(1-16) sequence formed in H₂O were investigated using electrospray ionization mass spectrometry (MS) and tandem MS (MS/MS). Aβ16 monomers and dimers were indicated by signals representing multiple proton adduct forms, [monomer+zH]ⁿ⁺ (=M^z+, z = charge state) and [dimer+zH]^z+ (=D^z+), in the MS spectrum. Fragment ions of monomers and dimers were observed using collision-induced dissociation MS/MS. Peptide bond dissociation was mostly observed in the D1-D7 and V11-K16 regions of the MS/MS spectra for the monomer (or dimer), regardless of the monomer (or dimer) charge state. Both covalent and non-covalent bond dissociation processes were indicated by the MS/MS results for the dimers. During the non-covalent bond dissociation process, the D³⁺ dimer complex was separated into two components: the M¹⁺ and M²⁺ subunits. During the covalent bond dissociation of the D³⁺ dimer complex, the b and y fragment ions attached to the monomer, (M+b_10-15)^z+ and (M+y_9-15)^z+, were thought to originate from the dissociation of the M²⁺ monomer component of the (M¹⁺+M²⁺) complex. Two different D³⁺ complex geometries exist; two distinguished interaction geometries resulting from interactions between the M¹⁺ monomer and two different regions of M²⁺ (the N-terminus and C-terminus) are proposed. Intricate fragmentation patterns were observed in the MS/MS spectrum of the D⁵⁺ complex. The complicated nature of the MS/MS spectrum is attributable to the coexistence of two D⁵⁺ configurations, (M¹⁺+M⁴⁺) and (M²⁺M³⁺), in the Aβ16 solution.