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.

In this study, the calibration characteristics of six new odorant VOCs along with two reference compound were evaluated based on GC-MS (SIM). For the proper evaluation of the GC/MS method, calibration of 7 VOCs were made both by the SPME and direct injection (DI). The minimum detection limit (MDL) of those VOC determined by SPME method fell in the range of 0.31∼0.38 ppb while those of DI from 6.18∼14.3 ppb. The analytical performance of our SPME/GC-MS method was compared against those tested previously by other study groups. Although more efforts are needed to establish the reliability of our SPME/GC-MS method, the method adapted in this study can be recommended as one of the standard methods for the analysis of the target VOCs in this study to settle formal experiment methods.

A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination (R2) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300㎍/L. The relative standard deviations were 3.4 and 2.1% for concentration of 10㎍/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and 1.3㎍/L, respectively.

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.