본 연구는 패류 독소 중 기억상실성 독성을 유발하는 domoic acid의 분석법 개선, 검증 및 분석적용성을 살펴보 았다. SAX 카트리지 정제, 검체 및 추출용매 양의 변경 과 더불어 이동상을 용매구매 조건으로 변경시킨 분석법 은 지중해담치, 홍게 그리고 멸치의 세 가지 매트릭스를 대상으로 세 농도에 대하여 식품공전법과 비교하여 유효 성을 검증하였다. 그 결과 변경된 분석법은 LOD 0.02-0.03 mg/kg, LOQ 0.05-0.09 mg/kg, 일내 및 일간 정확도 86.2- 100.4%와 일내 및 일간 정밀도 0.2-4.0%로 CODEX가이 드라인을 만족하는 우수한 분석능을 나타내었다. 특히 변 경된 시험법에서는 domoic acid와 유사한 머무름 시간을 갖는 방해물질이 검출되지 않아 위양성 결과를 방지할 수 있을 것으로 생각된다. 더 나아가 본 분석법이 국내 유통 중인 수산물을 대상으로 적용될 수 있는지 확인하고자 식 품공전의 기억상실성 패독 분석법과 함께 수산물에 적용 하여 분석하였다. 그 결과 5종의 수산물 87건 중 공전시 험법으로 분석했을 때 domoic acid가 검출된 시료는 없었 으나 변경된 분석법을 통하여 멸치 1건에 대하여 0.14 mg/ kg의 domoic acid이 미량 검출되었다. 따라서 본 연구에 서 확립된 분석법은 수산물 중 domoic acid 분석에 활용 이 가능할 것으로 보인다.

The methods for determining the diffusion parameters for the diffusion of d-limonene, a major volatile compound of orange juice, through a multi-layered food packaging material and predicting its absorption into the packaging material have been investigated. The packaging material used was the 1.5-mm thick multi-layered packaging material composed of high impact polystyrene (HIPS), polyvinylidene chloride (PVDC), and low density polyethylene (LDPE). Orange juice was placed in a cell where volatiles were absorbed in the sample package and kept at 23±2oC for 72 hr. The d-limonene absorbed in a 1.5-mm thick multi-layered food packaging material was analyzed by a solid phase micro-extraction (SPME). The absorption parameters for the absorption of d-limonene in the packaging material were determined and absorption of d-limonene into the packaging material was predicted using absorption storage data. The SPME desorption at 60oC for 1 hr resulted in the most sensitive and reproducible results. The diffusion coefficients of d-limonene in the packaging material and the partition coefficient at 23±2oC were approximately 1-2×10-12m2/s and 0.03, respectively. The absorption profile no earlier than 30 hr was fit well by a model derived from the Fick’s law.

The pomegranate (Punica granatum), especially its fruit, possesses a vast ethnomedical history and represents a phytochemical reservoir of heuristic medical value. The tree and fruit can be divided into several anatomical compartments, and the fruit juice, peel and oil are known to be weakly estrogenic and heuristically of interest for treatment of menopausal symptoms and sequellae. In this study, analysis of estrogen in pomegranate extract was carried out with LC/MS/MS. Three batches of pomegranate extract samples were used to analysis the target compounds (estrogen). The contents of estrogen derivatives in the samples were 38.6 ppb of estriol, 83.5 ppb of estrone,and 10.9 ppb of estradiol. This result suggests that the pomegranate extract can used for treatment of menopause symptoms in the woman.

Solid phase micro extraction(SPME)법의 최적조건 실험 및 SPME로 추출된 산초(Zanthoxylum schinifolium)의 휘발성 성분을 GC/MSD로 확인하였다. 휘발성 성분 추출에 자주 이용되는 동시증류추출(SDE)법으로 산초의 휘발성분을 분석하여 SP-ME 법에서 확인된 휘발성 성분과 조성비를 비교하였다. SPME 최적조건 시험에서 분자량이 적고 비점이 낮은 성분은 온도가 증가할수록 화이버에 흡착되는 양은 적게 나타났으며, 분자량이 크고 비점이 높은 성분은 추출시간이 증가할수록 흡착되는 양은 증가하였다. SPME 최적조건인 추출시간 30분과 50℃에서 분리된 휘발성 성분에서는 limonene(14.65%), geranyl acetate(11.07%), β-phellandrene(7.42%), 및 phellandral(3.08%) 등의 monoterpenoids 화합물과 caproic acid(11.99%), caprylic acid(8.01%), heptanoic acid(3.49%) 등의 지방산 화합물이 주요 성분으로 확인되었고, SDE법으로 추출된 휘발성 성분에서는 geranyl acetate(13.31%), limonene(12.81%) β-phellandrene(8.86%), trans-geraniol(5.22%) 및 caprylic acid(3.03%) 등의 화합물이 주요 성분으로 확인되었다. 지방산 성분들은 SPME법에서 높게 나타난 반면에 알코올 성분들은 SDE법보다 낮았다. SPME법은 적은 양의 시료로도 매우 신속하고 간단하게 전처리 할 수 있기 때문에 기존의 휘발성분 분석시 주로 사용한 SDE법에 비해 편리하며 경제적인 것으로 생각된다.

A simple, rapid and simultaneous analytical method is described for the detection of Sulfonamide and Tetracycline residues, i.e., Sulfamerazine (SMR), Sulfamethazine (SMT), Sulfamonomethoxine (SMM), Sulfadimethoxine (SDM), Sulfaquinoxaline (SQN), Oxytetracycline (OXY), Tetracycline (TC), Chlortetracycline (CTC). Blank control and sulfonamide and tetracycline fortified fish muscle samples (0.5 g) were blended with octadecylsilyl (C,e, 40 gm, 21% load, 60Å) derivatized silica packing material (2 g). Blended fish samples were washed with hexane, then, benzene and dichloromethane were used for the elution of tetracycline and sulfonamide, respectively, The eluants containg tetracycline and sulfonamide were analyzed by HPLC. Correlation coefficients of standard curves for individual sulfonamide and tetracycline isolated from fortified samples were linear (0.9993±0.0003-0.9997±0.0003, 0.9493±0.078-0.9753±0.036), respectively, The average percentage recoveries of sulfonamide and tetracycline ranged as 80.86-96.52% to 85.88-92.23%, and 30.01-37.12% to 65.89-73.40%, for the concentration range (0.1--1.0 ppm) examined, respectively. Limit of detection for sulfonamide was 0. 05 ug/g, then, tetracycline was 0.1 ug/g. Detection of quantitation of sulfonamide residue was 0.0012 ppm for SMR in Paralichthys Odiuacleus and 0.0020 ppm for SMR, 0.015 ppm for SMM in Cyprinus Carpio. The applicability of this procedure is demonstrated by separation and detection of incurred tetracycline and sulfonamide residues in fish muscle tissue.

This study was conducted to compare the volatile flavor compounds of Artemisia annua L. after extraction by simultaneous steam distillation extraction (SDE) and solid-phase micro extraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis. Via SDE and SPME processes, 79 (1,254.00 mg/kg) and 39 (488.74 mg/kg) compounds were identified respectively. The compounds extracted by SDE included 27 alcohols, 13 aldehydes, 22 hydrocarbons, 3 esters, 12 ketones, 1 oxide and 1 N-containing compound, on the other hand, using the SPME method, 7 alcohols, 5 aldehydes, 1 ester, 18 hydrocarbons, 7 ketones, and 1 oxide were extracted. The major volatile flavor compounds of Artemisia annua L. isolated by the two methods were caryophyllene oxide, -caryophyllene, camphor, -selinene, -muurolene, 1,8-cineol, (E)-pinocarveol and pinocarvone. β β γ The sesquiterpene named caryophyllene oxide was the most abundant volatile flavor compound with relative contents of 234.16 mg/kg and 195.44 mg/kg obtained by the SDE and SPME methods, respectively. Among the identified volatiles, sabinene, β-pinene, α-terpinene, γ-terpinene, yomogi alcohol, myrtenol, (Z)-nerolidol, p-cymen-8-ol and eugenol were detected by the SDE method only while (E)-anethole and α-cubebene were detected by the SPME method only. This study confirmed that the composition and contents of the volatile flavor compounds vary between different extraction methods. More volatile flavor compounds were identified using the SDE method than the SPME method.

A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. 50/30 ㎛ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to 0.15 ㎍/L for VFAs and from 0.12 to 0.28 ㎍/L for indoles and the correlations observed (R2) were 0.975～1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.

The study was carried out to evaluate the new analytical method of phthalate esters(diethylphthalate, di-n -butylphthalate, butylbenzylphthalate, bis(2-ethylhexyl)phthalate), one of the endocrine disruptors, which were performed by GC/MS-SIM(selected ion monitoring). The phthalate esters were extracted from water samples using solid-phase extraction on C18 columns. It investigated that the extraction recovery rate of phthalate esters with different solvents and solvent volume. The optimal solvent was dichloromethane and proper volume of dichloromethane for recovery of phthalate esters was 4 mL. There were good linearities(above R2=0.9975) in the range 0.01～0.50㎎/L, and the detection limits were below 0.01～0.03㎍/L. The recovery rates, RSD and MDLs for phthalate esters were 80～114%, 5.0～8.1% and 0.03～0.11㎍/L, respectively. This method shows a good precision of phthalate esters.

SPME device was applied to determine the THM in an aqueous solution. The 6 kinds of THM was quantitatively detemined by using GC-ECD which has the sample extracted on the SPME fiber from an aqueous solution for 10 min. The THM components were well separated from CHCl_3 to the last CHBr_3 within 13 mans at the condition. 6 kinds of the volatile halogenated organic compounds: CHCl_3, CHBrCl_2, CHBr_2Cl, CHCl_3, C_2Cl_4, and CHBr_3, showed well defined calibration graph with good linearity from a few ppb level up to several tens of ppb concentration. CHBr_2Cl and C_2Cl_4, were detected from a few samples among the 10 of river samples. CHCl_3, however, was detected in 4 sea water samples with the highest of 10 ppb among the polluted 6 positions. Trace level of CHBr_2Cl and few ppb level of CHBr_3 were also detected at the other two sample stations. Most of the 13 rain water samples collected from 6 sampling stations were contained ppb level of CHCl_3, and also CHBr_2Cl, and C_2Cl_4 were only detected at trace level at a few rain samples among them. We could recognize the fact that our air and water environment has already been contaminated by certain volatile halogenated organic compounds through this study.