• Natural Product Sciences
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• 제20권4호
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• pp.243-250
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• 2014

A simple GC method with a FID detector was developed in order to determine two main compounds (${\beta}$-sitosterol and lupenone) for Adenophorae Radix. ${\beta}$-Sitosterol and lupenone were analyzed by the gradient thermal ramping method. Nitrogen was used as the carrier gas at 108 kPa. The flow rate of gas was 2.0 mL/min; $2{\mu}L$ of filtered sample was injected at a split ratio of 1 : 80. This method was fully validated with respect to linearity, precision, accuracy and robustness. Further, this GC-FID method was applied successfully in order to quantify two compounds in an Adenophorae Radix extract. The GC analytical method for classification analysis was performed by repeated analysis of 59 reference samples in order to differentiate between Adenophora triphylla var. japonica Hara and 14 Codonopsis lanceolata. The results indicate that the GC-FID method is suitable and reliable for the quality evaluation of Adenophorae Radix.

• Journal of Pharmaceutical Investigation
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• 제41권3호
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• pp.173-178
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• 2011

Injectable chitosan hydrogels have attracted great potential due to sustained-release property and safety. Here, palmityl-acylated glycol chitosan (Pal-GC) was used to generate physically cross-linked hydrogels by virtue of hydrophobic attraction of linear fatty carbons. Glycol chitosan was chemically modified with N-hydroxysuccinimide-activated palmitic acid in dimethylsulfoxide (DMSO) containing dimethylaminopyridine. Through a series of preparation steps of (i) dialysis with DMSO, (ii) addition of palmityl-acylated exendin-4 (Ex4-C16), and (iii) dialysis with water, Pal-GC was self-assembled to form physically cross-linked hydrogels entrapped with Ex4-C16. The Pal-GC derivative was analyzed by using 1H NMR, and the surface morphology of Pal-GC hydrogels formed was examined by scanning electron microscopy. Also, the hypoglycemic effect induced by Pal-GC hydrogels containing Ex4-C16 (250 nmol/kg) was evaluated in non-fasted type 2 diabetic db/db mice and compared with GC hydrogels containing native Ex4 at the same dose. Results showed that palmityl group was successfully conjugated with the amines of glycol chitosan, and that Pal-GC efficiently generated the hydrogels formation. Moreover, Pal-GC hydrogels containing Ex4-C16 was found to greatly prolong the hypoglycemia duration (~ 4 days). This was due to the dual-functions of the palmityl groups present in both GC and exendin-4 such as hydrophobic attraction and plasma albumin-binding. We consider this new type of self-assembled GC hydrogels loaded with Ex4-C16 would be a promising long-acting sustained-release system with anti-diabetic property.

• 약학회지
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• 제47권4호
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• pp.195-199
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• 2003

An analysis method for the determination of methylendedioxymethamphetamine (MDMA) and its metabolite methylendedioxymethamphetamine (MDA) in hair by gas chromatography/mass spectrometry was proposed. For MDMA and MDA analysis, hair samples were incubated in MeOH (1％ HCl), derivatized with trifluoroacetic anhydride and assayed by GC/MS. Hair of 18 subjects for drug abuse was analyzed for MDMA and MDA. Calibration curves for the determination of MDMA and MDA in hair showed a good linearity at a concentration range from 0.5 ng to 250 ng ($r^2$=0.999) The extraction recovery was determined from hair blanks at 50, 100 ng. The percentage of recovery were found to be 96.08∼103.48 with CV value of 1.62∼3.89. The concentrations of MDMA and MDA ranged 1.14∼38.06 ng/mg and 0.07∼3.91 ng/mg, respectively in 18 hair samples from MDMA abusers. The ratio of MDMA to MDA ranged from 9.65∼28.46 in all specimen. Hair analysis for MDMA is a useful method for identification of long-term drug abuser.

• 약학회지
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• 제37권4호
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• pp.356-361
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• 1993

A sensitive method for the determination of methamphetamine(MA) and amphetamine(AM) in hair was developed by gas chromatography/mass spectrometry using stable isotope-labeled internal standards, amphetamine-d$_{5}$ and methamphetamine-d$_{5}$. Hair sample was washed with MeOH, incubated with MeOH(I% HCI) overnight at $37^{\circ}C$ while stirring and extracted using solid phase extraction column on a vacuum manifold. The extract obtained was pentafluoropropionated, and applied to GC/MS. The calibration curves of MA and AM were linear from 2.5 to 250 ng (r>0.99 for both). The limit of detection was 0.1 ng/mg in hair and cut-off level was set at 0.25 ng/mg for both. Hair samples of 27 MA abusers showed positive results in the range 0.7 to 106.8 ng/mg. AM, its metabolite, was detected in 20 out of 27 samples. The ratio of MA versus AM was 4.6~38.3 in specimens. Hair analysis for methamphetamine by GC/MS is an effective method for identifying long-term drug abusers.

• 자원리싸이클링
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• 제15권5호
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• pp.11-16
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• 2006

폐 폴리스티렌과 모터 오일의 혼합물로부터 마이크로웨이브 열분해를 이용하여 유용한 고분자 원료물질의 회수를 위한 연구를 수행하였다. 마이크로웨이브 반응기로 quartz tube를 사용하였으며 마이크로웨이브 흡수체로 실리콘 카바이드를 사용하였다. 공정 변수로 마이크로웨이브 입력 파워를 180에서 250 W까지 변화시켰으며, 마이크로웨이브 조사시간을 30분에서 1시간까지 변화시키며 실험하였다. 열분해를 통하여 얻어진 생성물을 GC/MS를 사용하여 분석한 결과 스티렌, 메틸 스티렌, 톨루엔, 그리고 에틸벤젠이 4개의 주요 회수 성분이었으며, 이 중 폴리스티렌으로부터 스티렌의 회수율은 약 50% 이었다. 열분해에 마이크로웨이브를 사용함으로써 일반 열분해 보다 훨씬 낮은 온도에서 열분해가 이루어졌다.

• Natural Product Sciences
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• 제24권1호
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• pp.71-78
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• 2018

The present study deals with the determination of optimal values of operating parameters such as the temperature of heating, the mass of the plant material and the volume of water leading to the best yield of electromagnetic induction (EMI) heating extraction of Algerian Thymus fontanesii essential oil. After an appropriate choice of the three critical variables, eight experiments leaded to a mathematical model as a first-degree polynomial presenting the response function (yield) in the relation to the operating parameters. From the retained model, we were able to calculate the average response, the different effects and their interactions. The maximum of essential oil recovery percentage relative to the initial mass of plant material was 1.69%, and was obtained at ($140^{\circ}C$, 250 g and 4.5 L). The chemical composition of the Algerian T. fontanesii essential oil under the obtained optimal conditions ($140^{\circ}C$, 250 g and 4.5 L), determined by GC/MS and GC/FID, reveled of the presence of major components such as: carvacrol ($70.6{\pm}0.1%$), followed by p-cymene ($8.2{\pm}0.2%$).

• 한국식품영양과학회지
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• 제32권1호
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• pp.22-28
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• 2003

단삼을 건조시켜 분쇄한 후 methanol로 추출하여 여러 용매로 분획하여 식품부패미생물의 증식억제 효과를 검색하고 그 항균성 물질을 분리하였다. 단삼의 chloroform 분획 추출물은 B subtilis, S. aureus, L. monocytogenes. E. coli 및 V, parahaemolyticus에 대해서 가장 낮은 농도인 250 $\mu\textrm{g}$/disc 농도에서 가장 높은 항균활성을 나타내었다. 단삼의 chloroform 추출물을 silica gel coliumn chromatography와 TLC로 monitoring 하여 항균성을 실험하였다. 이 결과 우수한 항균성 을 보인 sub fraction을 재차 분리하여 붉은색 결정의 항균성 물질을 얻었고 이를 GC/MS, $^1$H-NMR, $^{13}$C-NMR 로 구조분석 한 결과 화학식 이 $C_{19}$ H$_{20}$ O$_3$이며 분자량이 296.141 의 cryptotanshinone으로 동정되었다.

• 한국식품저장유통학회지
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• 제1권1호
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• pp.1-7
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• 1994

To investigate the effect of several bactericides and fungicides against fruit & vegetable decay grapefruit seed extract(GFSE) was tested in a dilution solution. GFSE was shown to be effective against decay and rind breakdown and to extend the shelf-life of fruits and vegetables during storage and tiansport. Antimicrobial efficiency of GFSE on a wide spectra of gram + & - bacteria, moulds and yeasts was demonstrated by the measurement of minimal inhibitory concentrations performed (Bacteria 10-500ppm, Fungi:250-1,000ppm, Yeasts:100-250ppm). GFSE was separated and extracted into water-soluble fraction, water-insoluble and non-dialyzed fraction to isolate the antimicrobial substances. The water-soluble fraction showed the most active antimicrobial effect. The antimicrobial substances were isolated by gas chromatography. As the result of the isolation using GC, Peak-D was found to be the antimicrobial compound in GFSE. The identification of the most antimicrobial substance was carried out by using GC-MS.

• Mass Spectrometry Letters
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• 제12권2호
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• pp.31-40
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• 2021

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

• Restorative Dentistry and Endodontics
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• 제42권4호
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• pp.309-315
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• 2017

Objectives: This study assessed the effect of water storage on the flexural strength (FS) of low shrinkage composites. Materials and Methods: A total of 165 bar-shaped specimens ($2{\times}2{\times}25mm$) were fabricated of 2 low shrinkage composites (Filtek P90 [3M ESPE], GC Kalore [GC International]) and a conventional methacrylate-based composite (Filtek Z250 [3M ESPE]). The specimens were subjected to 3-point bending test at 6 time intervals, namely: immediately after curing, at 24 hours, 1 week, 1 month, 6 months, and 1 year following storage in wet and dry conditions. The FS of the specimens were measured by applying compressive load at a crosshead speed of 1.0 mm/min. Data was analyzed using 3-way analysis of variance (ANOVA) and Tukey's test. Results: Three-way ANOVA revealed significant interactions between time, type of composite, and storage condition (p = 0.001). Tukey's multiple comparison test revealed significant reductions in FS of all composites after 6 months and 1 year of storage in distilled water compared to dry condition. Conclusions: Filtek P90 showed the highest and GC Kalore showed the lowest FS after 1 year storage in distilled water. The immediate high strength of Filtek Z250 significantly decreased at 1 year and its final value was lower than that of Filtek P90.