• Journal of Pharmaceutical Investigation
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• 제22권3호
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• pp.197-204
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• 1992

A gas chromatographic method using nitrogen phosphorous selective detection was developed for simultaneous determination of haloperidol and its metabolite, reduced haloperidol, in human plasma. Combelen was used as internal standard, The method involved extraction and trimethylsilylation followed by the injection of $2-4\;{\mu}l$ of benzene layer, which was used to dissolve the trimethylsilylated derivatives of haloperidol and reduced haloperidol, onto SE-54 column [5% phenyl methyl silica fused capillary column, $16m{\times}0.22\;mm$ $(I.D.){\times}0.33\;{\mu}m$ (coated thickness)]. The temperature of column oven was programmed from $200^{\circ}C\;to\;300^{\circ}C$ at the increase rate of $10^{\circ}C/min and also the temperatures of injector and detector were set at $300^{\circ}C$. Helium was used as carrier gas and its flow rate was maintained at 30 ml/min. The detection was conducted with nitrogen phosphorous selective detector. The retention times for combelen, reduced haloperidol and haloperidol were found to be 9.14, 9.75 and 9.99 min, respectively. The detection limits for haloperidol and reduced haloperidol in human plasma were both 0.2 ng/ml. The coefficients of variation of the intra-assay were generally low (below 9.8%). The mean absolute recoveries of added haloperidol and reduced haloperidol from plasma were 72% and 84%, respectively. No interferences from endogenous substances were found.

• Applied Biological Chemistry
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• 제12권
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• pp.43-51
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• 1969

우리나라 주요 식품들의 단백질 아미노산 함량을 최근에 와서 크게 실용화되고 있는 GLC 방법에 의해 분석함에 있어서 GLC의 기술적 재평가를 하고자 시험 하였든바 1. 우선 여러식품들의 단백질 질소함량을 조사하여 GLC 분석에 필요한 시료량을 정하였으며 2. GLC에 주입한 17종 아미노산들이 대하여 조사한 결과 Arginine, Cystine, Histidine, Tyrosine을 제외한 13종만이 주입한 량에 비례하여 detector response 를 얻었다. 3. 13종 아미노산에 대한 RMR 치(値)를 얻었다. 4. 아미노산에 대한 recovery 검정(檢定)을 하였든바 거의 100% 가까이 recover되었으며, 가수분해가 recovery에 미치는 영향을 조사하였든바 별 영향이 없었음을 알았다. 5. GLC와 ion-exchange chromatography 분석법을 비교시험하였든바 백어포 시료에 있어서는 Threonine과 Asparagine만이 두 방법에서 거의 같게 나왔고 다른 아미노산들은 GLC에서 보다 많은량이 나타났다. 6. 각식품들에 대한 단백질 아미노산함량을 측정하였든바 식품종류에 따라 그리고 보리 및 대두에 있어서는 품종에 따라서도 아미노산 함량이 다르게 나타났다.

• 한국식품과학회지
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• 제20권5호
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• pp.732-735
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• 1988

식용유의 향미 안정성을 측정하기 위하여 가스크로마토그래피를 이용하여 유지시료의 윗 공간내에 있는 총 휘발성물질, 산소 및 수소의 양을 측정하였다. 유지의 산패가 진행됨에 따라 총 휘발성물질의 양과 수소의 양은 유의적으로 증가하였으며, 두 값 사이의 상관계수는 0.95이상으로 높게 나타났다. 이러한 상관관계는 유지의 향미 안정성을 측정하기 위하여 가스크로마토그래피를 반복하여 실험할 필요없이 시료 윗 공간내의 수소와 산소의 양을 한 칼럼을 사용하여 동시에 측정함으로써 유지의 향미안정성을 나타내는 지료로써 수소와 산소의 함량이 사용될 수 있음을 시사하였다.

• 한국식품과학회지
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• 제4권1호
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• pp.24-28
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• 1972

Synthetic food preservatives were analysed in foods collected in Seoul area on Aug. 10, 1971. Sorbic acid, benzoic acid, dehydroacetic acid and butyl p-hydroxybenzoate were determined by the simultaneous gas chromatography using FID at $200{\circ}C$ and a column of Chromosorb W coated with 5% $DGS{\sim}1%\;H_3PO_4$. The recovery rates of each preservative were from 76.7% to 96.3%. The calibration curves show linearity within a range from 0.3 to $2.5{\mu}g$ of standard preservatives. The results obtained were as follows: 1) Benzoic acid was used as well as butyl p-hydroxybenzoate in soy. 2) Sorbic acid was not found in soy. 3) From all breads and biscuits benzoic acid was found as trace. 4) Detected preservatives were below the range of permitted limit. 5) From 2 soy among 15 samples dehydroacetic acid was found.

• Bulletin of the Korean Chemical Society
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• 제26권4호
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• pp.529-536
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• 2005

Measurement of toxicologically relevant polychlorinated biphenyl (PCB) congeners such as non-ortho(IUPAC#) 77, 81, 126, 169 and mono-ortho 105, 114, 118, 123, 156, 157, 189 and di-ortho 170, 180 and polybrominated diphenyl ethers (PBDEs) such as 47, 66, 85, 99, 100, 138, 153, 154 in environmental samples become almost mandatory in several countries now. However, most of the available methods involve expensive instrumentations such as HRGC-HRMS or ECNI-LRMS, apart from expensive extraction and clean-up (with large volume of solvents) steps. A method has been devised combining the analytical separation power of PYE [2-(1-pyrenyl)ethyldimethysilylated silica] column HPLC and high-resolution gas chromatographic techniques including micro-electron capture detection (ECD) and two dimensional gas chromatograpy-ECD techniques to determine these eco-toxic substances at parts-per-trillion (ppt) levels. This combination resolves co-elution of congeners that occur in disproportionate ratios (e.g. CB-110 and -77) and allows accurate congener-specific determination of target compounds. This method is cost effective as it requires only hexane, that in small quantities (10 mL) and GC-ECD. The elution and analysis time are optimized to less man hours. This method is effectively utilized in the analysis of co-planar PCBs and PBDEs from archived solvent extracts of samples previously analyzed for pesticides and PCBs. Structure based separation of contaminant classes improves GCECD determination at ppt levels.

• 한국식품위생안전성학회지
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• 제9권1호
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• pp.1-13
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• 1994

A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

• 한국식품과학회지
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• 제25권4호
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• pp.299-306
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• 1993

본 연구에서는 일부 한국산 식품의 식이섬유 함량을 Englyst 등의 비색법과 gas chromatography 방법에 의한 비전분 다당류 분석에 의하여 측정하였다. Gas chromatography 방법에 의한 비전분다당류의 측정 결과, 곡류와 두류의 비전분다당류에서는 glucose와 5탄당인 arabinose 및 xylose, 미역, 다시마와 채소류의 불용성 비전분 다당류에서는 glucose, 수용성 비전분 다당류에는 uronic acid가 주요당이었다. 또한, 김의 불용성 및 수용성 비전분 다당류에는 galactose가 상당량 함유되어 있었다. Englyst와 Cummings의 비색법(x)과 gas chromatography 방법(y)에 의한 비전분다당류 값의 상관관계는 곡류, 두류 및 채소류의 식품군에서 y=1.01x-0.52(r=0.997, n=9)로 좋은 일치를 보여주었다. 한편 AOAC 공정법에 의한 총 식이섬유 함량(x)과 Englyst와 Cummings의 gas chromatography 방법에 의한 비전분 다당류 함량(y)의 상관관계 y=0.55x+2.14(r=0.786, n=12)로서 상관관계가 낮았으나, AOAC 공정법에 의한 총 식이섬유 함량(x)과 비전분 다당류 함량에 lignin 함량을 합한 값(y)의 상관관계는 y=0.68x+0.64(r=0.903, n=12)이었다.

• 한국연초학회지
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• 제36권1호
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• pp.26-33
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• 2014

Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

• 한국식품과학회지
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• 제16권2호
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• pp.242-250
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• 1984

간장 80종에서 각각(各各) 간장 향기성분(香氣成分)을 용매 추출하여 gas chromatogram을 얻어 이 간장 향기(香氣)의 gas chromatogram 상의 자료를 변수변환(變數變換)하고 이와 관능검사(官能檢査) 점수와의 관계를 중회귀분석법(重回歸分析法)에 의해 해석하였다. 각 peak치(値)와 관능검사(官能檢査) 점수와의 단일상관은 전체적으로 낮고, 최고의 peak는 10번과 12번으로 0.331이었다. 각 변수변환(變數變換)에 의한 해석 정도는 비슷했다. 단계적 중회귀분석(重回歸分析)을 행한 결과(結果) 절대치(絶對値)에서는 step 16에서 간장 향기(香氣)의 약 56% 이상을 설명(說明)할 수 있었다. 단체적(團體的) 중회귀분석(重回歸分析)에 있어서 표준추정(標準推定) 오차(誤差)는 step 16에서 최소치(最小値)를 나타냈다. 이것은 F비의 결과(結果)와 함께 추정정도(推定程度)에 대(對)해 변수선택의 중요성(重要性)을 나타낸다. 각 peak에 있어서 기여율을 통해 보면 peak 10, 12번이 한국재래식(韓國在來式) 간장 향기(香氣)의 양부에 결정적인 역할을 하고 있다고 생각된다.

• Environmental Analysis Health and Toxicology
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• 제17권2호
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• pp.141-145
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• 2002

Benfuresate의 잔류분석을 위해 GC-FPD(S-mode)를 이용하여 분석조건을 설정 중 열적 불안정으로 인해 열분해 산물과 모 화합물이 혼재됨이 확인되었다. 가스크로마토그라프를 이용한 열분해의 주된 요인은 주입구의 온도와 주입구내의 기화 정도인 것으로 판단되었으며, 주입구를 Chauhan과 Debre 가 고안한 on-column으로 교체 후 분석한 결과 분해산물이 없는 단일 봉우리의 크로마토그램을 얻을 수 있었고, 절대량으로 0.6-4ng의 정량 범위 내에서 유의성 높은 검량선을 얻을 수 있는 주입구 온도는 20$0^{\circ}C$였다.