• 상하수도학회지
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• 제18권6호
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• pp.731-741
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• 2004

The purpose of this study was to evaluate the potential of a gamma ray irradiation to decompose hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in an aqueous solution. The decomposition reaction of RDX by gamma ray irradiation was a first-order kinetic over the applied initial concentrations (10-40mg/L). The dose constant was strongly dependent on the initial concentration of the RDX. The removal of RDX was more efficient at pH below 3 and at pH above 11 than at neutral pH (pH 5-9). The required irradiation dose to remove 99% of the RDX (40mg/L) was 4, 8 and 1 kGy, at pH 2, 7 and 13, respectively. The dose constant was increased by two folds and over twelve folds at pH 2 and 13, respectively, when compared with that at pH 7. When an irradiation dose of 20 kGy was applied, the removal efficiencies of TOC were 80, 57 and 91% at pH 2, 7 and 13, respectively. Ammonia and nitrate were detected as the main nitrogen byproducts of RDX and formic acid was detected as an organic byproduct. The results showed that a gamma ray irradiation was an attractive method for the decomposition of RDX in an aqueous solution and it was found that a strong alkaline pH over 12 should be applied to the decomposition reaction of RDX.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3284-3288
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• 2013

This paper describes first development and validation of pentafluorophenylprophyl ligand-based liquid chromatography coupled to tandem mass spectrometry (PFPLC-MS/MS) method to determine metformin, a highly polar compound, in human plasma. Metformin and Phenformin (internal standard) were extracted from human plasma 50 ${\mu}L$ with a single-step protein precipitation. The chromatographic separation was performed using a linear gradient elution of mobile phase involving 5.0 mM ammonium formate solution with 0.1% formic acid (A) and acetonitrile (B) over 3.0 min of run time on a Phenomenex Luna PFP column. The detection was performed using a triple-quadrupole tandem mass spectrometer (Waters Quattro micro) with electrospray ionization in the mode of positive ionization and multiple-reaction monitoring (MRM). The developed method was validated with 5.0 ng/mL of lower limit of quantification (LLOQ). The calibration curve was linear over 5-3000 ng/mL of the concentration range ($R^2$ > 0.99). The specificity, selectivity, carry-over effect, precision, accuracy and stability of the method met the acceptance criteria. The method developed in this study had had rapidness, simplicity and ruggedness. The reliable method was successfully applied to high throughput analysis of real samples for a practical purpose of a pharmacokinetic study.

• Bulletin of the Korean Chemical Society
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• 제30권1호
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• pp.137-144
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• 2009

In this study, quantitative and pattern recognition analyses for the quality evaluation of Herba Epimedii using HPLC was developed. For quantitative analysis, five major bioactive constituents, hyperin, epimedin A, epimedin B, epimedin C, and icariin were determined. Analysis was carried out on Capcell pak $C_{18}$ column ($250{\time}4.6$ mm, 5 ${\mu}m$) with a mobile phase of mixture of acetonitrile and 0.1% formic acid, using UV detection at 270 nm. The linear behavior was observed over the investigated concentration range (2-50 ${\mu}g/mL;\;r_2\;>$ 0.99) for all analytes. The intraand inter-day precisions were lower than 4.3% (as a relative standard deviation, RSD) and accuracies between 95.1% and 104.4%. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of one reference sample. The RSD of intra- and inter-day variation of relative retention time (RRT) and relative peak area (RPA) of the 12 selected common peaks were below 0.8% and 4.7%, respectively. The developed methods were applied to analysis of twenty Herba Epimedii extract samples. Contents of hyperin, epimedin A, epimedin B, epimedin C, and icariin were calculated to be 0$\sim$0.79, 0.69$\sim$1.91, 0.93$\sim$9.58, 0.65$\sim$3.05, and 2.43$\sim$11.8 mg/g dried plant. Principal component analysis (PCA) showed that most samples were clustered together with the reference samples but several apart from the main cluster in the PC score plot, indicating differences in overall chemical composition between two clusters. The present study suggests that quantitative determination of marker compounds combined with pattern-recognition method can provide a comprehensive approach for the quality assessment of herbal medicines.

• 분석과학
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• 제28권4호
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• pp.299-307
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• 2015

In May 2012, a safety hazard issue arose because some kiwifruit growers in New Zealand had sprayed streptomycin to prevent kiwifruit canker. Therefore, for food safety management, analytical methods to determine streptomycin residues in kiwifruits are required. We developed an analytical method to determine streptomycin residues in kiwifruit samples using liquid chromatograph tandem mass spectrometer (LC-ESI-MS/MS). Streptomycin residues in samples were extracted using 1% formic acid in methanol, centrifugation for 10 min, and subsequent supernatant filtration. Purified samples were subjected to LC-ESI-MS/MS to confirm presence of and quantify streptomycin residues. Average streptomycin recoveries (6 replicates each sample) were in the range of 94.8%-110.6% with relative standard deviations of <10%. The linearity of the concentration range of 0.01-5.0 mg/kg using a matrix-matched calibration gave R² = 0.9995. The limit of quantification (LOQ) was 0.01 mg/kg. Results showed that our analytical method is rapid, simple, and sensitive, with easy sample preparation.

• Asian-Australasian Journal of Animal Sciences
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• 제20권3호
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• pp.378-384
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• 2007

Three microorganisms and one chemical preservative were tested for their effects on the fermentation and aerobic stability of whole-crop wheat, sorghum and maize silages. Wheat at the early dough stage, sorghum at the late milk stage and maize at the one-third milk line stage were harvested and ensiled in 1.5-l anaerobic jars untreated or after the following treatments: control (no additives); Lactobacillus plantarum (LP) at $1.0{\times}10^6$ colony-forming units (CFU)/g of fresh forage; L. buchneri (LB) at $1.0{\times}10^6$ CFU/g; Propionibacterium acidipropionici (PA) at $1.0{\times}10^6$ CFU/g; and a formic acid-based preservative (FAP) at 3 ml/kg of fresh forage weight. Three jars per treatment were sampled on d 90 after ensiling, for chemical and microbiological analysis. At the end of the ensiling period, 90 d, the silages were subjected to an aerobic stability test lasting 5 d. In this test, $CO_2$ produced during aerobic exposure was measured along with chemical and microbiological parameters which serve as spoilage indicators. The silages inoculated with LP had higher concentration of lactic acid compared with the controls and the other treated silages (p<0.05). The controls and LP-inoculated silages spoiled upon aerobic exposure faster than LB, PA and FAP-treated silages. The controls and LP-inoculated silages spoiled upon aerobic exposure faster than LB, PA and FAP-treated silages due to more $CO_2$ production (p<0.05) in these two groups and development of yeasts unlike the other groups. In the experiment, the silages treated with LB, PA and FAP were stable under aerobic conditions. However, the numbers of yeasts was higher in the LP-inoculated wheat, sorghum and maize silages compared with the LB, PA and FAP-treated silages. The LB, PA and FAP improved the aerobic stability of the silages by causing more extensive heterolactic fermentation that resulted in the silages with high levels of acetic and propionic acid. The use of LB, PA and FAP as silage additives can improve the aerobic stability of whole-crop wheat, sorghum and maize silages by inhibition of yeast activity.

• 보존과학회지
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• 제30권4호
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• pp.353-364
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• 2014

포름알데히드는 전시 수장 공간에서 농도와 발생빈도가 높아 전통직물(천연염색)에 대한 손상 개연성이 있다. 본 연구는 견, 면, 모시, 삼베의 무염색, 천연염색(적색, 황색, 청색, 흑색) 시편을 대상으로 포름알데히드 0.5, 1, 10, 100, 500ppm 농도에서의 손상, 손상농도 500ppm에서 온습도 조건에 따른 손상과 열화상태에서의 손상을 광학적, 화학적, 물리적 측정방법으로 평가하였다. 이 결과, 포름알데히드 농도 500ppm에서 일부 직물의 색차, 변퇴색등급, 포름산이온 농도, pH가 변화하였으며, 고온 고습조건($30^{\circ}C$, 80%), 고습조건($25^{\circ}C$, 80%)에서는 색차, 변퇴색등급, 포름산이온 농도가 2배 가중되었다. 그러나, 열화직물은 열화정도, 열화 생성물질로 인해 포름알데히드에 의한 손상변화가 미미하였다. 이를 통해 포름알데히드에 의한 전통직물의 손상, 손상농도, 손상가중 조건, 열화상태에서의 손상을 확인하였으며, 포름알데히드는 적색직물의 황변, 열화직물의 황변 탈색, 포름산은 전체직물의 탈색에 영향을 미치는 것으로 나타났다.

• Journal of Ginseng Research
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• 제32권4호
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• pp.390-396
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• 2008

For evaluating the quality of ginseng, simple and fast analysis methods are needed to determine the ginsenoside content of the ginseng products. The aim of this study was therefore to optimize conditions for fast analysis of the ginsenosides, the active ingredients in extracts of Korean red ginseng. When tandem HPLC mass spectrometry (HPLC-MS/MS) was used, four forms of ginsenoside, Rb1, Rb2, Rc, and Re, were readily separated in seven minutes using a gradient mobile phase (acetonitrile and water containing acetic acid). This is the shortest separation time reported among the studies of major ginsenoside analysis. When gradient HPLC with UV detection was used, the detection limit was high, but separation of these four ginsenosides required 25 minutes using acetonitrile and water containing formic acid as a mobile phase. HPLC-MS/MS was able to separate ginsenoside Rg1 easily regardless of the mobile phase condition, but the HPLC-UV could not separate Rg1 because acetonitrile concentration in the mobile phase had to be maintained below 20%. Ginsenoside peaks were clearer and had more sensitive detection limits when Korean red ginseng extract was analyzed by the HPLC-MS/MS, but the UV detection was useful for chromatographic fingerprinting of all four major ginsenosides of the extract: Rb1, Rb2, Rc, and Re. Extracts were found to contain 2.17 mg, 1.51 mg, 1.29 mg, and 0.46 mg of ginsenoside Rb1, Rb2, Rc, Re, respectively, per gram weight. The ratios of each ginsenoside in the extracts were 1.0 : 0.7 : 0.6 : 0.2, respectively. Taken together, the results indicate that HPLC-MS/MS spectrometry could be the most useful method for rapid analysis of even small amounts of major ginsenosides, while HPLC with UV detection could also be used for rapid analysis of major ginsenosides and for quality control of ginseng products.

• 한국환경농학회지
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• 제34권2호
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• pp.105-110
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• 2015

BACKGROUND: Soy isoflavones, structurally similar to endogenous estrogens, may affect human body through both hormonally mediated and non-hormonally related mechanisms. Heat processing could change chemical compositions. The effects of different thermal processes, boiling and HTHP(high temperature and high pressure) on the composition of isoflavone compounds and total amount of domestic soybeans were investigated in this study. METHOD AND RESULTS: Three different kinds of soybean samples were collected from RDA-Genebank. The samples were extracted using methanol, distilled water, and formic acid based solvent. Also the same solvents were used for mobile phase in UPLC/ToF/MS. All of the isoflavone compounds were analyzed based on the aglycone type of external standard for quantification. The standard calibration curve presented linearity with the correlation coefficient R2 > 0.98, analysed from 1 to 50 ppm concentration. The total isoflavone contents does not change by treatment within the same breed. While "boiling" and "HTHP" processes tend to increase the contents of aglycone and ${beta}$-glucosides, "fresh" soybeans retained the high concentration of malonylglucosides. CONCLUSION: These results have to be considered while developing an effective functional food, from the health while point of view using soybeans.

• 한국식품위생안전성학회지
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• 제29권2호
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• pp.131-140
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• 2014

본 연구에서는 LC-MS/MS를 이용하여 페니실린계 동물용의약품 8종, 암피실린, 아목시실린, 클록사실린, 디클록사실린, 나프실린, 옥사실린, 페니실린 G, 페니실린 V의 동시분석법을 확립하고 잔류실태조사를 수행하였다. 피페라실린을 내부표준물질으로 적용하였으며, 이동상으로는 0.05% 포름산 용액와 0.05% 포름산 아세토니트릴 용액을 gradient mode로 사용하였고 $C_{18}$ 칼럼을 이용하여 분석하였다. 각 분석물질은 MRL의 0.25, 0.5, 1, 2, 4, 8배 농도범위에서 검량선을 작성하여 $R^2{\geq}0.99$의 직선성 및 재현성을 확인하였다. 소고기, 돼지고기, 닭고기에 대하여 MRL의 0.5, 1, 2배인 세 가지 농도에서 6회 반복으로 분석을 실시한 결과, 평균 회수율은 71.0~106%, 상대표준편차는 4.0~11.2%, LOD는 0.003~0.008 mg/kg, LOQ는 0.01~0.03 mg/kg이었다. 국내 유통 소고기, 돼지고기, 닭고기에서 페니실린계 항생제 8종의 분석결과, 총 193건 중 경기도 지역의 국내산 소고기 1건에 대해서 클록사실린이 MRL 이하인 0.08 mg/kg이 검출되었으며, 나머지 192건의 검체에서는 불검출로 분석되었다. 본 연구를 통하여 확립된 페니실린계 동물용의약품 8종 동시분석법은 식육에 대한 페니실린계 동물용의약품의 안전관리 체계 방안을 제시하기 위한 기초자료로 활용 가능한 것으로 사료된다.

• Journal of Pharmaceutical Investigation
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• 제37권4호
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• pp.223-227
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• 2007

A rapid, simple and sensitive LC/MS/MS method for the determination of lercanidipine in human serum was validated and applied to the pharmacokinetic study of lercanidipine. Lercanidipine and internal standard, amlodipine, were extracted from human serum by liquid-liquid extraction with hexan-isoamyl alcohol (100: 1, v/v) and analyzed on a $Symmetry^{(R)}$ MS $C_{18}$ column with the mobile phase of acetonitrile-0.2% aqueous formic acid (70: 30, v/v). Using MS/MS with multiple reaction monitoring (MRM) mode, lercanidipine and amlodipine were detected without severe interferences from human serum matrix. Lercanidipine produced a protonated precursor ion ($[M+H]^+$) at m/z 612.3 and a corresponding product ion at m/z 280.0. Internal standard produced a protonated precursor ion ($[M+H]^+$]) at m/z 409.0 and a corresponding product ion at m/z 238.0. The ruggedness of this method was investigated using quality control (QC) samples. This method showed linear response over the concentration range of 0.05-20 ng/mL with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 mL of serum was 0.05 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the developed method ranged from 85.51 to 112.2% for lercanidipine with overall precision (% C.V.) being 3.56-13.1%. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of lercanidipine in human serum samples for the pharmacokinetic studies, demonstrating the suitability of the method.