• Journal of Food Hygiene and Safety
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• v.16 no.1
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• pp.61-65
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• 2001

To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

• The Korean Journal of Pesticide Science
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• v.9 no.2
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• pp.159-165
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• 2005

A sensitive derivatization method by using the TFE/TFAA as derivative reagent is proposed for the determination of acidic herbicides in water, by using this method, method detection limits are improved by 10 times and sample volumes are decreased by 5 times compared with other methods such as U.S. EPA and SPEED 98. And also, in order to suggest higher creditable standard operating procedure (SOP), intra- and inter-lab validation test carried out by four laboratories include our lab. The results of intra and inter-lab validations in same experimental conditions show good linearity in given range of concentrations as a $0.1{\sim}10.0$ ng/ml, and range of accuracies and precisions show $-20.5{\sim}12.2$ bias%, $0.55{\sim}24.48%$ (for intra-lab validation) and $-6.66{\sim}0.80 bias%$, $1.92{\sim}13.86%$ (for inter-lab validation), respectively.

• Analytical Science and Technology
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• v.9 no.2
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• pp.198-202
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• 1996

A rapid and simple method for the determination of histamine by reverse-phase high performance liquid chromatography with fluorescence detection was established. 9-Fluorenylmethyl chloroformate(FMOC) was used as fluorescent derivative reagent. The optimum conditions for the derivatization such as pH, reaction time and the concentration of FMOC were investigated. Linearity of calibration curve was obtained between $0.1{\mu}g/ml$ and $0.5{\mu}g/ml$(r=0.992) and the limit of detection was $0.01{\mu}g/ml$.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 2008.11a
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• pp.248-251
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• 2008

일반적으로 phthalate esters의 전처리방법에는 액액추출법(liquid-liquid extraction), 고상추출법(Solid-phase Extraction, SPE), 고상미세추출법(Solid-phase micro extraction, SPME) 등의 분석방법이 있다. 그 중에서 본 연구에서는 SPE를 이용하여 간편하고 정확성이 높으며, 적은 양의 유기용제를 사용하여 전처리함으로써 2차적인 환경오염을 줄일 수 있다는 점에서 다른 전처리 방법보다 유용하다고 할 수 있다. 검출감도 측면에서 phthalate esters의 경우는 구조적으로 안정적인 편이나 페놀류의 경우 hydroxy group 때문에 GC/MS 분석시 유도체화 과정이 필수적인데 이번 연구에서 사용한 BSTFA/TMCS는 비교적 쉽고 빠르게 유도체 화할 수 있다는 이점이 있다. 더 많은 연구가 필요하겠지만 앞서서의 결과에서도 알 수 있듯이 전반적으로 검출한계가 0.05$\sim$0.5 $\mu$g/L 정도로 높고, 4-nonyl phenol을 제외하고 80% 이상의 양호한 회수율을 나타낸 것으로 미루어 보아 phthalate esters, phenols의 효율적인 동시분석이 가능함을 알 수 있다.

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
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• 2005.10a
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• pp.196-203
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• 2005

축산식품 고기내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발 을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/Dihydro streptomycin, Neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법 등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 DST에 대한 HPLC법에 대한 보고한 P. Edder 방법 중에 clean-up과정 및 이동상 조건을 대폭 수정하여 DST의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering Laboratories, Inc.)의 컬럼온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, reagent 유속 0.6ml/min mobile phase 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 DST 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 DST의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection (LOD)은 0.02ppm이었으며, 적어도 고기에서의 MRL이 0.6ppm임을 감안하면 DST를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 고기에 표준 DST를 1ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 DST의 limit of quantification(LOQ)는 약 0.47ppm이었으며, 이에 대한 회수율은 97.7%(n= 8)를 나타냈다. 실제 codex에서 권장한 고기의 MRL이 0.6ppm인 점을 감안하면 codex 권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발된 시험법은 지금까지 국내적으로 DST에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 DST에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 DST에 대한 분석시험법의 개발이 가능하다고 여겨진다.

• Analytical Science and Technology
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• v.12 no.1
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• pp.28-33
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• 1999

Glutathione(GSH) in biological samples was determined by high performance liquid chromatographic(HPLC) method with fluorescence detector(FLD) after monobromobimane(MBB) or 4-fluoro-7-sulfobenzofurazan(SBD-F) derivatization. The detection limit of $0.03{\mu}g/mL$ was obtained after MBB derivatization, derivative of MBB was about 200 times more sensitive than that of SBD-F. N-acetylcysteine was used as internal standard and tetrabutylammonium ion as counter ion for better separation. The determination by ion-pairing chromatography after MBB derivatization was characterized by linearity in the range between $0.08{\sim}8.33{\mu}g/mL$ with a good correlation coefficient of 0.998. By precision test appeared relative standard deviation at less than 5% at three different concentrations. This method can be used for the analysis of GSH in plasma and tissue.

• Analytical Science and Technology
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• v.13 no.4
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• pp.484-493
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• 2000

The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

• Analytical Science and Technology
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• v.21 no.6
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• pp.543-552
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• 2008

This paper described the relatively sensitive and simultaneous analytical method for 3-monochloropropane-1,2-diol (3-MCDP, $C_3H_7ClO_2$, MW. 110) as well as 1,3-dichloropropan-2-ol (1,3-DCP, $C_3H_6Cl_2O$, MW. 128) in various foods. Food samples were homogenized in 5M NaCl solution, mixed with aluminum oxide and eluted with dichloromethane. The extracted chloropropanols were concentrated by rotary evaporator and $N_2$ blow serially were derivatized with HFBA (Heptafluorobutyric anhydride, $C_8F_{14}O_3$, MW. 410) and were determined by GC/MS using isotope dilution method. The characteristic molecular ions at m/z 253, 275, 289, 291, and 453 for HFBA derivatives of 3-MCPD (MW. 502) and 110, 275, and 277 for HFBA derivatives of 1,3-DCP (MW. 325) were chosen in selected ion mode. The method validation data showed sufficiently good properties of LOD (0.003 mg/kg), LOQ (0.010 mg/kg), linearity ($R^2{\geq}0.999$ at 0.010~1.000 mg/kg), and recovery rate (${\approx}97%$). The levels of chloropropanols in soy sauce, sauces, processed meat products, fishery products, and seasonings (n=56/157) determined by the presented method were 0.0~0.3 mg/kg.

• Journal of the Korean Chemical Society
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• v.52 no.3
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• pp.239-248
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• 2008

study of the solid phase extraction (SPE) technique using activated carbon fiber (ACF) as a sorbent was carried out on the schedule chemicals in water. 14 different schedule chemicals, which are the hydrolysis products and simulants of chemical agents such as alkylphosphonate, thiodiglycol etc. were selected for the study. Pyridine was used as a promoter to increase the derivatization efficiency, especially to improve silylation of 3-quinuclidinol. To improve the recovery efficiency of amines in the water solution, 1 mL of 5% Et3N/MeOH was introduced into SPE-ACF before the water sample loading. Throughout this study, the optimum condition was established to detect rapidly above chemicals in water.

• Analytical Science and Technology
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• v.20 no.5
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• pp.400-405
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• 2007

The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.