• Mass Spectrometry Letters
• /
• 제12권1호
• /
• pp.21-25
• /
• 2021

We aimed to develop and validate a sensitive analytical method of nannozinone A, active metabolite of Nannochelins A extracted from the Myxobacterium Nannocytis pusilla, in mouse plasma using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Mouse plasma samples containing nannozinone A and 13C-caffeine (internal standard) were extracted using a liquid-liquid extraction (LLE) method with methyl tert-butyl ether. Standard calibration curves were linear in the concentration range of 1 - 1000 ng/mL (r2 > 0.998) with the inter- and intra-day accuracy and precision results less than 15%. LLE method gave results in the high and reproducible extraction recovery in the range of 78.00-81.08% with limited matrix effect in the range of 70.56-96.49%. The pharmacokinetics of nannozinone A after intravenous injection (5 mg/kg) and oral administration (30 mg/kg) of nannozinone A were investigated using the validated LC-MS/MS analysis of nannozinone A. The absolute oral bioavailability of nannozinone A was 8.82%. Plasma concentration of nannozinone A after the intravenous injection sharply decreased for 4 h but plasma concentration of orally administered nannozinone A showed fast distribution and slow elimination for 24 h. In conclusion, we successfully applied this newly developed sensitive LC-MS/MS analytical method of nannozinone A to the pharmacokinetic evaluation of this compound. This method can be useful for further studies on the pharmacokinetic optimization and evaluating the druggability of nannozinone A including its efficacy and toxicity.

• Mass Spectrometry Letters
• /
• 제12권1호
• /
• pp.16-20
• /
• 2021

We aimed to compare the content of ginsenosides and the pharmacokinetics after the oral administration of four different ginseng products at a dose of 1 g/kg in rats. The four different ginseng products were fresh ginseng extract, red ginseng extract, white ginseng extract, and saponin enriched white ginseng extract prepared from the radix of Panax ginseng C.A. Meyer. The ginsenoside concentrations in the ginseng product and the rat plasma samples were determined using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Eight or nine ginsenosides of the 15 tested ginsenosides were detected; however, the content and total ginsenosides varied depending on the preparation method. Moreover, the content of triglycosylated ginsenosides was higher than that of diglycosylated ginsenosides, and deglycosylated ginsenosides were not present in any preparation. After the single oral administrations of four different ginseng products in rats, only four ginsenosides, such as 20(S)-ginsenosides Rb1 (GRb1), GRb2, GRc, and GRd, were detected in the rat plasma samples among the 15 ginsenosides tested. The plasma concentrations of GRb1, GRb2, GRc, and GRd were different depends on the preparation method but pharmacokinetic features of the four ginseng products were similar. In conclusion, a good correlation between the area under the concentration curve and the content of GRb1, GRb2, and GRc, but not GRd, in the ginseng products was identified and it might be the result of their higher content and intestinal biotransformation of the ginseng product.

• Mass Spectrometry Letters
• /
• 제13권4호
• /
• pp.166-176
• /
• 2022

Banana peels are also widely used as bio-adsorbent in the removal of chemicals contaminants and heavy metals from water and soil. GC-MS plays an essential role in the phytochemical analysis and chemo taxonomic studies of medicinal plants containing biologically active components. Intrinsically, with the use of the flame ionization detector and the electron capture detector which have very high sensitivities, Gas chromatography can quantitatively determine materials present at very low concentrations and most important application is in pollution studies. In the present study banana peels were used as bio-adsorbent to remediate the heavy metal contaminated water taken from three different stations located around the industrial belts of Ranipet, Tamilnadu, India. The AAS analysis of the samples shows a decrement of chromium concentration of 98.93%, 96.16% and 96.5% in Station 1, 2 and 3 respectively which proves the efficiency of the powdered peels of Musa paradisiaca. The GC-MS analysis of the control and treated peels of Musa paradisiaca reveals the presence of phytochemicals like Acetic Acid, 1-Methylethyl Ester, DL-Glyceraldehyde Dimer, N-Hexadecanoic Acid, 3-Decyn-2-Ol, 26-Hydroxy, Cholesterol, Ergost-25-Ene-3,5,6,12-Tetrol, (3.Beta.,5.Alpha.,6.Beta.,12.Beta.)-, 1-Methylene-2b-Hydroxymethyl-3, and 3-Dimethyl-4b-(3-Methylbut-2-Enyl)-Cyclohexane in the control banana peels. The banana peels which were used for the treatment reveals the changes and alteration of the phytochemicals. It is concluded that the alteration in phytochemicals of the experimental banana peels were due to adsorption of chromium heavy metal from the sample.

• Mass Spectrometry Letters
• /
• 제2권4호
• /
• pp.92-95
• /
• 2011

Pyrophosphates are the key intermediates in the biosynthesis of isoprenoids, and their concentrations could reveal the benefits of statins in cardiovascular diseases. Quantitative analysis of five pyrophosphates, including isopentenyl pyrophosphate (IPP), dimethylallyl pyrophosphate (DMAPP), geranyl pyrophosphate (GPP), farnesyl pyrophosphate (FPP), and geranylgeranyl pyrophosphate (GGPP), was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative ionization mode. After dilution with methanol, samples were separated on a 3 ${\mu}m$ particle multi-modal $C_{18}$ column ($50{\times}2$ mm) and quantified within 10 min. The gradient elution consists of 10 mM ammonium bicarbonate and 0.5% triethylamine (TEA) in water and 0.1% TEA in 80% acetonitrile was used at the flow rate of 0.4 mL/min. Overall recoveries were 51.4-106.6%, while the limit of quantification was 0.05 ${\mu}g$/mL for GPP and FPP and 0.1 ${\mu}g$/mL for IPP, DMAPP, and GGPP. The precision (% CV) and accuracy (% bias) of the assay were 1.9-12.3% and 89.6-111.8%, respectively, in 0.05-10 ${\mu}g$/mL calibration ranges ($R^2$ > 0.993). The devised LC-MS/MS technique with the multi-modal $C_{18}$ column can be used to estimate the biological activity of pyrophosphates in plasma and may be applicable to cardiovascular events with cholesterol metabolism as well as the drug efficacy of statins.

• Mass Spectrometry Letters
• /
• 제3권3호
• /
• pp.74-77
• /
• 2012

Organic acid (OA) profiling analysis was performed in culture media from Lactobacillus pentosus K34 (L. pentosus K34) and Pediococcus lolli PL24 (P. lolli PL24) by gas chromatography-mass spectrometry (GC-MS) following methoxime/tert-butyldimethylsilyl derivatives. 12 OAs were positively identified in culture media. Most of OA levels from L. pentosus K34 of hetero lactic fermentation were found to be higher when compared with those from P. lolli PL24 of homo lactic fermentation, which may explain different OA metabolism in each strain. In addition, the distorted dodecagonal star patterns were readily distinguishable, and the characteristics of each strain were well represented. The present study demonstrates that the OA metabolic profiling method by GC-MS combined with star pattern recognition is useful for the monitoring study of characteristic OA metabolism in various microorganisms.

• 한국표면공학회지
• /
• 제31권1호
• /
• pp.12-23
• /
• 1998

The Thermal Barrier Coating(TBC) has been used to improve the heat barrier and tribological properties of the aircraft engine and the automobile engine in high temperature. Especially, the high temperature tribological propertied of the cylinder haed and the piston crown of diesel engine was emphasized. Therefore, the purpose of this work was to evaluate the microstructure, tribological propeer in high tempearmal shock resistance and bonding strength of five layer functionally gradient TBC for the applications. The five layerwere composed with 100% ceramic insulating later, 75(ceramic):25 (metal) layer, 50:50 layer, 25:75 layer and 100% metal bonding layer to redude the thermal stress. the YSL and MSL poweders were the insulation ceramics powers. The NiCrAly, Inconel625 and SUS powders were the bonding and mixingg powders for plasma spray process. According to the result of high temperature wear test, the wera resistance of YSZ/NiCrAlY siytem was most out standing at 600 and $800^{\circ}C$. At $400^{\circ}C$, the wear resistance of YSZ/Inconel system was better than others. Wear volume at other temperature because of the low temperature degration of zirconia. The thermal shock mechanism of 5 later is the vertical crack gegration in insulating layer. this means that the initial cracks were generated in the top layer, and then developed into the composite layers during thermal shock test. Finally, these cracks werereached to the interface of coating and substrate and also, these vertioal cracks join with the horizontal cracks of the each layers. The bonding strength of YSZ/NiCrAlY and YSZ/Inconel 5 layer system is better than other 5layer systems. The theramal shock resistance of thermal barrier coating s with 5 layer system is better than that of 3 layers and 2 layers.

• Mass Spectrometry Letters
• /
• 제10권2호
• /
• pp.66-70
• /
• 2019

Rivaroxaban (RRN) is the first available active direct factor Xa inhibitor (anticoagulant) with oral administration. Due to its success in market, there have been efforts to develop various RRN formulations, and the development of good analytical methods for its in vivo evaluation is an essential prerequisite. Thus, here, a simple and efficient method to determine RRN in rat plasma using liquid-liquid extraction (LLE) and liquid chromatography and multiple reaction monitoring (LC-MRM) was presented. The use of ethyl acetate as the LLE solvent results appropriate extraction and purification of RRN and it also helps the significant reduction of rat plasma volume required for RRN quantitation. The developed method showed good analytical performance including specificity, linearity ($r^2{\geq}0.999$ within 0.5 - 500 ng/mL), sensitivity (the lower limit of quantitation at 0.5 ng/mL), accuracy (89.3 - 107.0%), precision (${\geq}12.7%$), and recovery (89.2 - 105.7%). Additionally, RRN in sample extracts showed good stability. Finally, the applicability of the validated method to the PK evaluation of RRN was confirmed after its oral administration to normal rats. The present method is the first analytical method employing LLE for the simple and efficient extraction and purification of RRN in rat plasma. Therefore, the present method can contribute to the development of new RRN formulations as well as to the monitoring of RRN in special clinical situations through its efficient determination in various samples with or without minor modification.

• Mass Spectrometry Letters
• /
• 제13권4호
• /
• pp.133-138
• /
• 2022

Taurine is a type of sulfur-containing amino acid having a sulfate functional group, that is biosynthesized from cysteine. It is mainly distributed in high concentrations in animal tissues and is known to have various effects such as osmotic pressure control, calcium control, anti-inflammatory, antioxidant, and hepatocellular protection. Also, taurine deficiency causes a variety of symptoms, including visual impairment. In particular, in the case of cats, taurine is not biosynthesized and must be supplied through food, so it is classified as an essential amino acid. In this study, an analysis method using mass spectrometry was developed instead of the commonly used derivatization method to quickly, environmentally, and precisely analyze taurine in various animal feeds. The developed analytical method showed good linearity (R² > 0.99), accuracy (81.97-105.78%), and precision (0.07-12.37%). In addition, the developed method was further verified through quantitative comparison with the derivatization method. This developed method was used in the determination of taurine in 20 animal feed samples obtained from South Korea. The levels of taurine found ranged from 81.53 to 6,743.53 mg/kg. The developed analysis method will be used for the detection and quantification of taurine in domestic feed.

• Mass Spectrometry Letters
• /
• 제13권3호
• /
• pp.58-83
• /
• 2022

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL^-1; linearity (r²) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL^-1, linearity (r²) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

• 대한토목학회논문집
• /
• 제3권1호
• /
• pp.1-12
• /
• 1983

자연해안(自然海岸)에 호안등(護岸等) 구조물(構造物)과 새로운 용지(用地)의 확보(確保)를 위해 매립(埋立)을 행(行)하였을 경우 이에 수반되는 예기(豫期)치 않던 지형변화(地形變化) 해안공학상(海岸工學上) 커다란 문제점(問題點)으로 대두(擡頭)되고 있다. 본(本) 연구(硏究)는 최근(最近) 사빈침식(砂濱侵蝕)이 심(甚)하게 얼어나고 있는 해운대사빈(海雲臺砂濱)의 침식방지(侵蝕防止) 및 양빈공법(養濱工法)을 모색(摸索)할 목적(目的)으로 사빈(砂濱)의 단면변화특성(斷面變化特性)을 안정적(安定的)으로 진단(診斷)하고자 하였으며 다음과 같은 해석방법(解析方法)에 의해 진단(診斷)을 행(行)하였다. (1) 현장실측자료(現場實測資料)에 의해 사질단면(砂質斷面)의 경년적변화(徑年的變化)를 조사(調査)하였다. (2) 저질특성(底質特性)에 의한 단면(斷面)의 형성(形成) 및 진행상태(進行狀態)를 고찰(考察)하였다. (3) Malkov chain model에 의한 이론적(理論的) 고찰방법(考察方法)을 해운대사빈(海雲臺砂濱)에 적용(適用)하고 단면(斷面)의 천이특성(遷移特性)을 한정(限定)된 단면형상(斷面形狀) 천이(遷移) model로 확정(確定)하여 단면변화(斷面變化)의 주행특성(走行特性)을 파악(把握)하였다. (4) 해운대사빈(海雲臺砂濱)의 천이(遷移) model 해석결과(解析結果)로서 매수면상(梅水面上)(MSL)의 저류표사량((貯溜漂砂量)을 확정(確定)하는 형상함수(形狀凾數)에 의해 결정(決定)된 자연사빈(自然砂濱)의 저류표사량산정식((貯溜漂砂量算定式)이 호안(護岸)과 같은 해안구조물(海岸構造物) 설치(設置)된 사빈단면砂濱(斷面) 저류표사량산정((貯溜漂砂量算定)에도 유용(有用)하게 적용(適用)될 수 있음을 검토확인(檢討確認)하였다.