• 대한약학회:학술대회논문집
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• 대한약학회 2001년도 Proceedings of International Convention of the Pharmaceutical Society of Korea
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• pp.286.2-286.2
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• 2001

• Preventive Nutrition and Food Science
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• 제7권1호
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• pp.12-17
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• 2002

Simultaneous determination of nine water-soluble vitamins contained in multi-nutrient tablets was carried out by reversed phase high-performance liquid chromatography (RP-HPLC) equipped with analytical $C_{18}$ column and UV (270 nm) detector. Those standard vitamins were successfully separated within 23 minutes by gradient elution with solvent A (0.5 M potassium phosphate monobasic) and solvent B (0.25 M potassium phosphate monobasic-methanol, 1:1). Calibration curves showed good linealities with correlation coefficients (> 0.92) in tested ranged respectively. The detection limits were considered to be 2.1 ng for ascorbic acids 60 ng for Vit B$_{6}$ 3 ng for p-aminobenzoic acid, 9 ng for niacinamide, 9 ng for thiamin, 5.0 ng for folic acid and 1.5 ng for riboflavin at 0.05 a.u.f.s. Solid phase extraction through Sep-Pak (C$_{18}$ ) cartridge was successfully applied for purification of water soluble vitamins in commercial multi-nutrient tablets.ts.

• 상하수도학회지
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• 제32권6호
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• pp.559-572
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• 2018

The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

• 한국물환경학회지
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• 제32권6호
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• pp.600-627
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• 2016

Korea is one of the countries with a large veterinary antibiotics market, although antimicrobial resistance in bacteria is becoming a serious issue in many countries. The Korean government started to take interest in estimating the effects of livestock manure on rivers and agricultural soils and in monitoring of heavy metals, organic pollutants and antibiotics in the ambient water and soil. In this paper, pre-treatment methods to separate the selected antibiotics from solid samples were reviewed. It is essential to select an efficient and appropriate procedure for pre-treatment due to the high proportion of proteins and organics in biosolid samples. Pre-treatment consists of extraction followed by clean-up. Initially, homogenized samples were extracted by sonication, mechanical agitation or pressurized liquid extraction with methanol/acetonitrile/water mixture under acidic/basic conditions depending on the compound. However, aminoglycosides and colistin were extracted with 5% trichloroacetic acid and HCl, respectively. Since the ${\beta}-lactams$ are easily decomposed in acidic and basic conditions, they were extracted in neutral pH. Filtration with a membrane (pore size, $0.2{\mu}m$) or solid phase extraction with HLB and methanol, as eluents, was normally applied for the clean-up. At least, three different pre-treatment procedures should be adopted to screen all the selected antibiotics in solid samples.

• 대한화학회지
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• 제52권3호
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• pp.239-248
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• 2008

활성탄소섬유(ACF; activated carbon fiber)를 흡착제로 사용한 고상추출법(SPE; solid phase extraction)으로 수용액 시료 중에 존재하는 특정화학물질(schedule chemicals)의 분석법을 연구하였다. 본 연구에 사용된 특정화학물질은 화학작용제류의 가수분해 생성물과 유사작용제로 사용되는 알킬포스포네이트류, 티오디글리콜 등 14종이었다. 분석을 위한 추출물의 실릴 유도체화 반응에서 피리딘을 사용하여 특히 3-quinuclidinol의 유도체화 반응 효율을 높일 수 있었다. 물 시료에서 아민류의 추출 회수율을 개선하기 위하여 SPE-ACF 튜브에 시료를 부하하기 전에 5% triethylamine/MeOH(1 mL) 용액으로 SPE-ACF 튜브를 세척한 후에 시료를 SPE-ACF에 부하하는 방법으로 추출 회수율을 증대시킬 수 있었다. 이 연구를 통해서 수용액 시료에서 특정화학물질을 신속히 검출할 수 있는 최적 조건을 선정하였다.

• Applied Biological Chemistry
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• 제42권3호
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• pp.210-217
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• 1999

전통민속주 제조에 이용되는 부재료 가운데 휘발성 향기성분인 asarone, coumarin, thujone등 식품에 허용기준이 제한된 독성 관련 향기성분을 함유하고 있는 식물성 방향재료 및 약용재료를 확인, 분류하기 위하여 이들의 20% ethanol 추출액으로부터 고상추출(solid phase extraction) 방법을 이용하여 각 성분을 흡착, 용리시킨 후 GC-FID와 GC/MS로 검출, 확인하였다. 조사대상 87종의 식물성재료 중 창포(Acorus asiaticus Nakai), 석창포(Acorus gramineus Solander), 당귀(Angelica gigus Nakai), 백단향(Santalum album) 등 6종에서 asarone이 검출되었으며, coumarin은 소회향(Anethum graveolens), 회향(Foeniculum vulgare Gaertner), 자초(Lithosperum erythrorhizon Siebold et Zuccarinii) 등 22종에서 검출되었다. 한편, 우실(Achyranthes japonica Nakai), 사인(Amomum xanthiodes Wallich), 약쑥(Artemisia asiatia Nakai), 대마자(Cannabis sativa L.)씨, 골담초(Caragana sinica R.), 국화(Chrysanthem morifolium Ramat), 사삼(Codonopsis lanceolata Bentham et flooker), 회향(Foeniculum vulgare Gaertner) 등 24종에서는 thujone을 확인하였다.

• 한국식품위생안전성학회:학술대회논문집
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• 한국식품위생안전성학회 2001년도 The Asia-Pacific Conference on Reproductive Biology and Environmental Sciences
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• pp.171-174
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• 2001

Solid phase micro-extraction (SPME), a solvent-free, rapid and inexpensive method for the extraction of organic compounds from aqueous sample matrices, was evaluated for determination of the 120 pesticides in vegetables such as crown daisy, perilla leaf, leafy lettuce and to mato. The analysis conditions were chosen for the SPME method: 15 min of immersion of the PDMS fiber in 10 ml of the solution with stirring at 1,000 rpm. The recovery tests were carried out in triplicate. The range of recoveries was 0-142% for organochlorine pesticides and $4.9\sim200\%$ for organophosphorus pesticides. The recoveries were very low in the pesticide groups with low solubility in water. The recoveries became lower in proportion to the interference materials in vegetables. The recovery in tomato was relatively higher than that in perilla Ie af and crown daisy. The recovery values obtained by SPE and SPME were compared. In leaf y lettuce, recovery obtained by SPE method ranged from $58.1\%\;to\;136.1\%$ and recovery by SPME ranged from $9.6\%\;to\;176.3\%$ In organophosphorus pesticides. The recovery in SPME method was satisfactory with $136\%$ for ethoprophos, $119\%$ for methidathion and $113\%$ for diazinon. Meanwhile, recovery of EPN, phenthoate and 2,4-DDT revealed relatively low value of $38\%,\;41\%\;and\;3.4\%,$ respectively. However, most of pesticides applied to SPME method sho wed constant recovery and precision. From these results, it can be concluded that solid phase micro-extraction might be an appropriate method for the screening test of pesticides in vegetables.

• Bulletin of the Korean Chemical Society
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• 제27권1호
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• pp.77-81
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• 2006

The commercially available Amberlite XAD-2 and XAD-4 resins were modified with macrocyclic protoporphyrin IX (PPIX) or tetrakis(p-carboxyphenyl) porphyrin (TCPP) to enhance the adsorption capacity for phenol and chlorophenols. The chemically modified polymeric adsorbents (XAD-2+PPIX, XAD-2+TCPP, XAD-4+PPIX, and XAD-4+TCPP) were applied to the solid phase extraction as an adsorbent material for the preconcentration of phenol and chlorophenols in environmental waters. Generally, the synthesized adsorbents showed higher recoveries than underivatized adsorbents, XAD-2 and XAD-4, without matrix interferences. Especially, XAD-4+PPIX showed more than 90% recoveries for all compounds used in this study including hydrophilic phenol. The major factor for the increase of the adsorption capacity was the increase of $\pi$-$\pi$ interaction between adsorbents and samples due to the introduction of the porphyrin molecule. However, the breakthrough volumes and recovery values of the XADs+TCPP columns were slightly decreased for the bulky chlorophenols such as TCP and PCP. Using molecular mechanics methods, the structures of TCPP and PPIX were compared with that of porphine, the parent molecule of porphyrin. Four bulky p-carboxyphenyl groups of TCPP were torsional each other, thus the molecular plane of TCPP were not on the same level. In conclusion, the decrease of breakthrough volumes and recovery values of XADs+TCPP columns for bulky phenols can be explained by the steric hindrance of the $\pi$-$\pi$ interaction between porphyrin plane and the phenols.

• 대한환경공학회지
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• 제35권2호
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• pp.75-83
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• 2013

본 연구는 기존의 고상추출(SPE) 과정을 분석장비인 LC/MSD에 on-line으로 연결함으로써 cartridge의 건조를 막아 target 물질의 손실을 최대한 억제하였으며 11종의 PFCs에 대해 실제 matrix가 있는 낙동강 원수를 이용한 실험에서 $80.4{\pm}5.2%{\sim}109.5{\pm}1.4%$ 범위의 높은 회수율을 구할 수 있었다. 낙동강에서의 PFCs 분포를 조사한 결과 하수처리장 방류수의 영향을 받는 지역(진천천과 금호강 하류)은 고농도의 PFCs가 검출되었으며, 낙동강 하류의 매리원수에서는 검출농도가 급격히 감소하여 PFOA만 8.0 ng/L의 농도로 검출되었다. 외국의 PFCs 검출현황을 보고한 연구결과들과 비교해 볼 때 낙동강 지류에서는 비교적 높은 농도로 PFCs가 검출되어 안심할 수 있는 수준은 아니었으며, 낙동강 본류의 경우도 여러 지역의 상수원으로 이용되기 때문에 주기적인 모니터링이 필요한 것으로 나타났다.

• Food Science and Biotechnology
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• 제18권6호
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• pp.1515-1518
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• 2009

The objective of this study was to compare 3 extraction methods including, solid phase extraction (SPE), acetonitrile extraction, and methanol extraction, for their usefulness as extraction methods to determine capsaicinoids. The determination of capsaicinoids in the extracts was carried out on a reverse-phased high performance liquid chromatography (HPLC) using a fluorescence detector. Three extraction methods, i.e., SPE, acetonitrile extraction, and methanol extraction were compared for the quantification of capsaicinoids using raw peppers and pepper powder. The highest analytical values were observed using methanol extraction and the lowest values using SPE. Also, the analytical method validation parameters such as accuracy, precision, limit of detection, limit of quantitation, and specificity were calculated to ensure the method's validity. This method provides a fast and accurate approach for the determination of capsaicinoids in peppers.