• 한국식품위생안전성학회지
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• 제18권2호
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• pp.43-50
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• 2003

A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

• Food Science and Biotechnology
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• 제14권2호
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• pp.249-254
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• 2005

The relationship between Sigumjang gas chromatographic patterns precisely analyzed with capillary column and ranked order in sensory analysis was investigated by stepwise multiple regression analysis. Highly predictable multiple regression models were obtained in the analysis. Ninety percent of the Sigumjang aroma was explained by the regression models at step 15 in four transformation except for absolute value transformed with root square and relative value transformed with logarithm. The aroma of Sigumjang was most affected by 2,3-dimethylpyrazine at absolute value and absolute value transformed with logarithm and by 2-furancarboxaldehyde in other transformation. The quality of sigumjang was highly affected by ${\beta}$-phallendrenal, methylpyrazine, tetramethylpyrazine, 5-methyl-2-furancarboxaldehyde, unknown 2, octanoic acid, 4-ethylphenol, methyl 10,13-octadecanoate and ethyl linoleate.

• Bulletin of the Korean Chemical Society
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• 제27권9호
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• pp.1315-1322
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• 2006

The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

• 분석과학
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• 제10권3호
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• pp.168-178
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• 1997

기체 크로마토그래피법을 이용하여 제초제인 ethalfluralin의 잔류분석을 위한 최적 측정 조건을 구하고, 토양에서의 잔류량과 반감기를 조사하였다. 토양시료를 methanol과 dichloromethane으로 추출하여 농축하였다. Toluene으로 다시 녹이고, cyanosilica gel 카트리지로 분리하여 전자포착형 검출기가 장착된 기체 크로마토그래프(GC-ECD)로 분석하였다. 0.1과 1.0ppm의 표준물을 첨가하였을 때, 92.8~101.2%의 회수율을 얻었으며, 검출한계는 0.004ppm이었다. Ethalfluraline의 반감기는 토양 (A)의 경우에는 실내에서 35일, 야외에서 7.2일이었으며, 토양 (B)의 경우에는 실내에서 45일, 야외에서 9.7일이었다.

• 분석과학
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• 제12권6호
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• pp.571-576
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• 1999

소변 시료에서 비스테로이드성 소염진통제 (Non-Steroidal Anti-Inflammatory Drugs)인 Fenamates 부류의 6종에 대해서 pentafluoropropionyl 유도체화 반응을 통하여 Gas Chromatograph/Negative Chemical Ionization-Mass Spectrometer에 감응도가 높은 유도체를 만들었다. 6종의 소염 진통제 약물에 대하여 반응성이 좋은 유도체화 반응 조건과 크로마토그래피 조건을 설정하였으며 이들 약물은 동시에 분석 가능하였고 검출한계가 4-25 pg/mL 이어서 경마 경기에서 자주 사용되고 있는 NSAIDs의 미량 성분에 대한 검출 및 법과학에서의 응용이 가능하다.

• Journal of Pharmaceutical Investigation
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• 제37권1호
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• pp.27-37
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• 2007

Proficiency test is an essential tool far ensuring analytical ability of analytical chemists and analytical institutes. Usually, the standard protocol for proficiency test is focused on acceptability of reported analytical results of participants by calculating z-scores and related diagnostic parameters. The ultimate goal of this process is to reveal the sources of variability of analytical results and to find the way to reduce their influence. In this study, the method of analysis of variance (ANOVA) was applied to the analytical data collected from qualify control departments of pharmaceutical companies in KyungIn province in Korea in the year of 2000. As influencing factors of variability of analytical results, the use of internal standards for liquid and gas chromatograpy, the educational and professional background of participants, geological locations and yearly production sizes of participating companies were evaluated. To evaluate the variability in accuracy of analytical results, absolute differences from sample mean and sample median were used and to evaluate variability in precision of individual participants, the reported standard deviation of each participant was used. As a result, the use of internal standards in gas chromatographic analysis, participants' academic background and the yearly production sizes of pharmaceutical companies showed statistically significant influence to the accuracy and the precision of the reported analytical results used in this study.

• Food Science and Biotechnology
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• 제14권5호
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• pp.656-660
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• 2005

The relationship between the gas chromatographic (GC) patterns of sauce made of barley bran and ranked order in sensory analysis was investigated by multiple regression analysis (MRA). Most of the 42 barley bran sauce samples comprised about 34 peaks, in which the content of 9, 12-octadecanoic acid methyl ester was the highest, followed by those of 2-furanmethanol and 2-furancarboxaldehyde. It is difficult to estimate the aroma quality of barley bran sauce samples on the basis of only one peak. The 34 aroma compounds of the 42 samples were analyzed by an MRA model featuring six transformations. The most precise fit was calculated from the absolute value transformed with the root square of each peak, and the multiple determination coefficient showed that 91.6% of the variation in the sensory score could be explained on the basis of GC data.

• 대한화학회지
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• 제30권5호
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• pp.465-474
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• 1986

농작물에 잔류되어 있는 11종의 유기인제 농약들을 추출하여 기체-액체 크로마토그래피로 동시에 분석함에 있어서 농작물별로 방해하는 다른 성분들을 분리, 제거하기 위한 액체-액체 분배와 컬럼크로마토그래피의 최적 조건을 찾고자 하였다. Acetone을 사용하여 농작물로부터 녹여낸 추출물에 포화 NaCl용액을 가하고 petroleum ether로 두 번 분배하여 농약들을 회수하였다. Activated carbon, magnesia 및 diatomaceous earth의 혼합 흡착제(1:2:4)를 충진시킨 컬럼에 petroleum ether에 분배된 추출물들을 넣고 methyl chloride로 용리시켰더니 가해준 농약의 82∼105%가 회수되었고 농작물에서 녹아나온 방해 성분들이 거의 제거되었다.

• 대한화학회지
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• 제38권10호
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• pp.726-733
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• 1994

대기부유분진(air particulate material)중에 존재하는 다환방향족탄화수소(polycyclic aromatic hydrocarbons, PAH)를 신속하고 정확하게 분석하기 위하여 대기부유분진 시료를 10ml의 초임계유체($N_2O$ )로 30분간 추출 후 별도의 전처리와 농축과정 없이 GC/MS에서 분석하여 분석시간과 분석과정을 단축 및 단순화하였다. 시료로서 NBS 대기부유분진 인증표준기준물질(certified particulate reference material, CRM)1649와 서울의 도심에서 채취한 대기부유분진 시료를 이용하여 기존의 추출법 및 분석방법과 비교하였다. 그 결과 본 분석방법은 기존의 분석법에 비해 회수율은 상대적으로 작았으나 재현성이 좋았으며 분석과정이 간단하고 분석시간이 현저히 단축됨을 알 수 있었다.

• 분석과학
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• 제8권4호
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• pp.739-744
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• 1995

The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.