• Journal of Pharmaceutical Investigation
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• 제12권4호
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• pp.126-131
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• 1982

A quantitative fluorometric method was developed to determine aspirin and salicylic acid in bulk aspirin and commercial aspirin tablets. The excitation maximum for aspirin was observed at 280 nm and the emission maximum was at 335nm. The lowest energy excitation band for salicylic acid was at 308nm and the fluorescence emission band was at 450nm. Excipients, binders, lubricants and impurities did not interfere. Excellent recoveries were obtained for aspirin and salicylic acid. Results obtained by the KP III procedure and the proposed method were compared.

• 한국환경독성학회:학술대회논문집
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• 한국환경독성학회 2003년도 추계국제학술대회
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• pp.149-149
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• 2003

A new technique is proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert.-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the GC/MS-SIM mode. The recoveries were 86.6∼105.2 % (isoBOC derivatization) and 97.6∼484.5 % (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol A for SIM were 0.001∼0.050 $\mu\textrm{g}$/l (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/l (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). The derivative methods and their application to tap water samples will be disscussed.

• 대한수의학회지
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• 제47권4호
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• pp.389-393
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• 2007

In this study, the levels of aflatoxin $M_1$ ($AFM_1$) in milk were determined by HPLC with derivatization method. Milk samples were purified using $C_{18}$ disposable cartridge followed by derivatization with trifluoroacetic acid and analysed using HPLC with fluorescence detection. The recoveries of AFM1 from milk samples added $AFM_1$ at a level of 0.025~0.1 ng/ml were 94.7~98.0% with detection limit of 0.009 ng/ml. The amounts of $AFM_1$ were determined below 0.05 ng/ml for all tested samples of commercial milk collected in 1999 and 2000.

• 한국식품위생안전성학회지
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• 제14권1호
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• pp.67-75
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• 1999

The new approach using the Peak Pattern Method was conducted for the analysis of polychlorinated biphenyls (PCBs) from the papers or paper products to provide certain hygienic data for the recycled papers as well as white papers. The height of the each peak, obtained from the PCBs standards, was transformed to the spectrum to compare with that of the samples. In addition to the results of the single PCBs standards, the pattern of mixed PCBs standards with the adequate concentration and ratios were obtained prior to the analysis of the paper samples. The test showed excellent repetition within 5% variation, and the recoveries of PCBs ranged from 92% to 97%. The PCBs, considered as a hazard material, were analyzed using the Peak Pattern Method from six different types of paper samples including the roll tissue. It could not find the same pattern of the PCBs peaks from all of the paper samples.

• 한국식품위생안전성학회지
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• 제12권3호
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• pp.210-216
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• 1997

The prevention of oxidative degradation in fats and oils is largely controlled by the use of synthetic phenolic antioxidants. Antioxidants, BHA: 2-&-3-tert-butyl-4-hydroxyanisol, BHT: 3,5-di-tert-butyl-4-hydroxytoluene, TBHQ: tert-butylhydroquinone, PG: propyl gallate, PTG: pentyl gallate, OG:octyl gallate, were extracted from fatty foods with hexane and from hexane layer to presaturated acetonitrile with hexane. The polar phenolic hydroxyl groups of antioxidants were silylated with MSTFA and injected to Gas Chromatography/Mass Spectrometry. The calibration plots were linear in the investigated range, 0.1~10.0 $\mu\textrm{g}$/g. The limit of detection for 6 phenolic antioxidants was 0.1 $\mu\textrm{g}$/g. Recoveries and reproducibilities from samples fortified at 1.0 $\mu\textrm{g}$/g were in the range of 70~90% and 0.5~13%, respectively. The simultaneous determination of phenolic antioxidants in fatty foods using GC/MS-SIM mode and macro program was described.

• Natural Product Sciences
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• 제17권2호
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• pp.104-107
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• 2011

In order to facilitate the quality control of betaine from the fruits of Lycium chinense, we have developed a rapid and simple method for quantitative determination. Determination was achieved on a Discovery C18 column with an isocratic solvent system of 0.32% perfluoropentanoic acid aqueous-acetonitrile at a flow-rate of 0.5 mL/min and detected an ELSD. The method was reproducible with intra- and inter-day variations of less than 6% (R.S.D). The recoveries were in the range of 90.01~100.05%. The method turned out to be fast and simple, furthermore, to have a good selectivity and sensitivity for the quantity determination of betaine in the fruits of L.chinense.

• 한국연초학회지
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• 제29권2호
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• pp.132-139
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• 2007

This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

• Journal of Applied Biological Chemistry
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• 제43권2호
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• pp.94-100
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• 2000

An analytical method was developed to determine abamectin and milbemectin residues in apple, pear, and citrus using HPLC with ultraviolet absorption detection. Abamectin and milbemectin were extracted with methanol from apple, pear, and citrus samples. The extract was diluted with saline water and dichloromethane partition was followed to recover the compounds from the aqueous phase. Florisil column chromatography and aminopropyl solid-phase extraction were employed as cleanup methods to remove most of co-extractives from the sample extract. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate abamectin and milbemectin residues in sample extracts at the wavelength of 245 nm. Recoveries of abamectin and milbemectin from fortified samples ranged 80.4~90.3% and 90.9~96.8%, respectively. Relative standard deviations of the analytical method were less than 10% for both acaricides. Detection limit of the analytical method was 0.003 mg/kg sample for all the analytes. The proposed method was reproducible and sensitive enough to evaluate terminal residues of abamectin and milbemectin in apple, pear, and citrus.

• 분석과학
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• 제16권6호
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• pp.438-442
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• 2003

본 연구에서는 우리나라에서 시판되고 있는 국내 및 외제 와인에 대하여 vinclozolin, dichlofluanid, penconazole, procymidone 등의 살균제 잔류함량을 고체상 추출법을 이용한 GC/MS-SIM 방법으로 정량 하였다. 분석결과 모든 시료에서 procymidone의 함량이 $2.2-76.1{\mu}g/L$가 검출되었고, 회수율은 81.3-93.1 %, 표준편차는 1.4-3.4 %로 나타났다.

• 분석과학
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• 제8권4호
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• pp.535-538
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• 1995

This study employs the variety of mixtures of XAD resin and active carbons as concentration base for solid phase extraction (SPE) which has been widely used to preconcentrate and purify phenol and chlorophenols in determination of environmental water samples. In this study, we employed variety of mixtures of copolymer based XAD-4 resin with active carbons. This cartridges shows advantages of both materials, such as better affinity to phenol by active carbon and better mechanical stabilities from XAD resin. The better enrichment factor, pretreatment time, recoveries and limit of detection (LOD) were achieved by the attempts to pack precolumns with both meterials for preconcentration.