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.

A study of the tissue depletion of florfenicol (FFC) administered orally to pigs at a dose of 0.05 kg/ton feed for 7 days was performed. Sixteen healthy cross swine were administered with FFC. Four treated animals were arbitrarily selected to be sacrificed 1, 3 and 5 days after the end of treatment. FFC residue concentrations in muscle, liver, kidney, and fat were determined using high-performance liquid chromatography (HPLC) with ultraviolet photometric detector at 230 nm. The correlation coefficient (R2) of the calibration curve for florfenicol amine (FFCa) was > 0.997 and the limits of detection and quantification were 0.012 and 0.040 μg/mL, respectively. Recovery rates in swine edible tissues ranged from 79.1 to 93.5%. In the FFC-treated group, FFC residues at 3 days post-treatment were below the maximum residue limits (MRLs) in muscle, kidney and fat, and those at 5 days post-administration were below the MRLs in all edible tissues. These results suggest that the withdrawal period of FFC after the drug treatment might be 5 days, which is a sufficient amount of time for reduction of the FFC residues below the MRLs in all edible tissues.

본 연구에서는 식품용 기구 및 용기·포장으로부터 식품유사용매로 이행되는 12종의 자외선흡수제(Uvinul 3000, Cyasorb UV 24, Uvinul 3040, Tinuvin 312 및 P, Seesorb 202, Chimassorb 81, Tinuvin 329, 234, 326, 328 및 327) 의 분석법을 확립하였다. 식품유사용매 중 물, 4% 초산, 50% 에탄올의 경우 hydrophilic-lipophilic balance (HLB) 카트리지로 고체상 추출법(Solid Phase Extraction)을 이용 하였고, n-헵탄의 경우 이소프로판올로 희석하여 HPLCUVD (310 nm)로 자외선흡수제의 이행량을 분석하였다. 확 립된 분석법으로 일회용기, 밀폐용기, 일회용백, 소스병, 물병, 도시락 등 국내 유통 폴리에틸렌(60건) 및 폴리프로 필렌(140건) 재질의 식품용 기구 및 용기·포장 200건으로부터 식품유사용매로 이행되는 12종의 자외선흡수제 이행량 조사 결과, 물, 4% 초산, 50% 에탄올, n-헵탄 4가지 식품유사용매 모두에서 자외선흡수제는 검출되지 않았다. 따라서, 실제 가정에서 폴리에틸렌이나 폴리프로필렌 재 질의 식품용 기구 및 용기·포장을 사용하는 환경에서는 자외선흡수제의 이행 정도는 안전한 수준인 것으로 판단 된다. 또한, 자외선흡수제를 0.1 wt%, 0.5 wt%씩 첨가하여 제작한 시편에서의 이행정도는 0.02~0.5% 수준으로 나타나 통상적인 식품용 기구 및 용기·포장을 사용하는 조건에서 자외선흡수제의 이행량은 크지 않은 것으로 나타났고, 안전한 수준임을 확인할 수 있었다. 본 연구에서 확립 된 12종 자외선흡수제의 식품유사용매로의 이행량 동시분 석법은 폴리에틸렌 및 폴리프로필렌 식품용 기구 및 용 기·포장의 안전관리를 위한 기초자료로 활용될 수 있을 것으로 기대된다.

Oxathiapiprolin은 병원균의 포자형성과 효모성장을 저해하여 노균병을 방제하는 piperidinyl thiazole isoxazoline 계열 살균제로 2015년 국내 사용등록이 요청된 신규약제이다. 본 연구에서는 oxathiapiprolin의 신규등록과 관련해 안전관리를 위한 공정시험법 마련이 요구되어 농산물 중 잔류분석법을 개발하였다. 농산물 중 oxathiapiprolin은 acetonitrile로 추출한 뒤 분배효율 향상을 위해 1 N sodium hydroxide (NaOH)를 이용해 염기성으로 조절하여 비해리상태로 만든 뒤 dichloromethane으로 액액분배하였으며 분배추출액은 silica SPE 카트리지로 정제한 뒤 HPLC-UVD로 분석하였다. 개발된 분석법의 검출한계(LOD) 및 정량한계(LOQ)는 각각 0.003, 0.01 mg/kg이었고, 대표농산물 5종(고추, 감귤, 감자, 대두, 현미) 중 oxathiapiprolin의 평균 회수율은 86.7-112.7%(상대표준편차, RSD ≤ 10%)으로 나타났다. 이는 잔류물 분석에 관한 CODEX 가이드라인 (CAC/GL 40)을 만족하는 것으로 확인되었다. 따라서 개발된 분석법은 국내외 유통 농산물 중 oxathiapiprolin의 안전평가를 위한 잔류량 적부 판정에 있어 공정시험법으로 사용되기에 적합할 것으로 판단된다.

Background : Alpinia Officinarum Rhizome (高良薑) is recorded as a roots of Alpinia officinarum Hance (Zingiberaceae) in Korea Pharmacopoeia and there is no established confirmation test and method for quantitative determination using marker compound. Using the six marker compounds, pinocembrin, (5S)-5-hydroxy-7- (4-hydroxy-3-methoxyphenyl) -1-phenyl-3-heptanone, pinocembrin, galangin, kaemferide, galangin 3-methyl ether, A simultaneous analysis method was developed to utilize the quality control. Methods and Results : In this study, YMC-pack column (ODS C18, 250 × 4.6 ㎜, 5 ㎛) from YMC was used and the temperature was set at 30℃. A soultion of 0.1% formic acid was using water (mobile phase A) and acetonitrile (mobile B), respectively, and the mobile phase B was set to 15 - 35% for 0 - 15 minutes and 35 - 40% for 15 - 60 minutes. And 270 ㎚ was set as the detection wavelength. The order of the components is pinocembrin (1, Rt: 23.2 min), (5S)-5-hydroxy-7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-heptanone (2, Rt: 37.8 min), pinocembrin (3, Rt: 44.9 min), galangin (4, Rt: 46.7 min), kaemferide (5, Rt: 48.6 min), galangin 3-methyl ether (6, Rt: 52.8 min) and Based on the retention time, ultraviolet spectrum and MS value, it was confirmed by comparison with standard compounds. Conclusion : In this study, we developed the simultaneous analysis method by six marker components of the Alpina officinarum Hance extract to develop a quality test method to scientifically identify Alpinia officinarum Hance.

Background : Coffee is one of the favorite brewed drink in the world where is distributed in Latin America, Southeast Asia, Southern Asia and Africa. Coffee has an effective antioxidant ability and reported about that. In this study, it was analyzed by using high performance liquid chromatography (HPLC) to establish the method about content of caffeine, chlorogenic acid, caffeic acid and p-coumaric acid in coffee. Methods and Results : Coffee was extracted with 70% EtOH in room temperature and evaporated at 45℃. All standard and sample extract were melted and diluted with 15% MeOH. Mobile phase was prepared using water with 0.01% phosphoric acid and MeOH. All standard and sample were analyzed with gradient elution (0 min : 15% MeOH, 35 min : 30% MeOH). The chromatograms were monitored at 272 and 320 ㎚. HPLC reported linear equation that based on the calibration curve for each standard compound (caffeine : Y = 1.04e + 004X – 3.21e + 003, R2 = 0.999890. chlorogenic acid : Y = 2.86e + 004X – 8.24e + 003, R2 = 0.999891. caffeic acid : Y = 2.07e + 004X – 1.21e + 004, R2 = 0.999894. p-coumaric acid : Y = 3.24e + 004X – 1.10e + 004, R2 = 0.999897). Standard compounds were determined with qualitative and quantitative analysis. The retention time of each peak of standard compounds were separated by chromatogram. Conclusion : In this study, we determined that the analysis method of compounds in coffee. In addition, we have confirmed that separation about the retention time of each peak of caffeine and chlorogenic acid in different solvent condition depending on acid buffer. This method can be use to determine standard compound in coffee.

A QuEChERS method was developed for the analysis of diazinon, chlorfenapyr, and lufenuron in Napa cabbage. These pesticides represent three different chemical classes and are commonly used in cabbage production in Korea. The objective of the proposed method is a fast, inexpensive, and easy extraction of pesticides, followed by rapid analysis. The proposed method involves a microscale extraction using acetonitrile and dispersive solid phase extraction (SPE), allowing for time and materials savings. The pesticides were separated and quantified using reversed-phase HPLC-UV at 220 nm. The calibration curves showed good linearity (R2>0.97), and the limits of detection and quantification were ≤0.05 and 1 mg/kg, respectively. Intraday and interday recoveries were in the range 97-116% and 101-112% with RSD% ≤9% for concentrations between 0.5-5 mg/kg. Abnormal recoveries and a substantial matrix effect were initially observed for lufenuron, signaling that optimization of lufenuron recovery requires a slight modification of the method. The proposed method was tested on cabbage samples sold at local markets, which showed no detectable residues of the target pesticides. The proposed method could thus be used for monitoring these pesticides in cabbage and similar vegetables.

Content analysis of loliolide in the leaves of Boehmeria nivea (Bn) collected from different region during four months (June, July, August, and September) was conducted by HPLC. The content of loliolide was detected in the leaves of B. nivea from Bns-2, -7, -10, -23, -38, -41, -67, -76, and -90 in June (5.02, 6.35, 6.93, 5.89, 4.31, 4.24, 4.91, 5.12, and 5.46 mg/g, respectively), July (4.32, 6.42, 7.72, 7.97, 4.05, 4.32, 5.65, 6.67, and 5.39 mg/g, respectively), August (3.52, 5.17, 3.90, 4.27, 3.26, 4.72, 3.82, 3.30, and 3.31 mg/g, respectively), and September (7.04, 7.25, 7.43, 7.86, 6.76, 6.38, 7.60, 6.79, and 4.77 mg/g, respectively). Among them, the highest content of loliolide was found in Bn-23 and in September. These results may be useful in determining the optimal harvest time at which phytochemical reaches a maximum level.

Sesamin and sesamolin, antioxidant lipidsoluble lignan compounds, are abundant in sesame (Sesamum indicum L.) seed oil and provide oxidative stability of oil related to sesame quality. The sesamin and sesamolin contents of 403 sesame land races of Korea were determined by HPLC analysis of methanol extract (HPLC value), and their total lignan content was compared with those by using UV-Vis spectrophotometric analysis (UV method) of methanol (UV-MeOH value) and hexane (UV-Hexane value) extracts. HPLC values of total lignan content were strongly associated with UV-Hexane (r=0.705**) and UV-MeOH (r=0.811**) values. The UV values from both the extracts were 3.8-4.7 times higher than those of HPLC values. Lignan content was overestimated by UV method because total compounds in the mixture solution were quantified by absorbing at the same ultraviolet wavelength as in HPLC method. UV method could more rapidly analyze small amount of sample with higher sensitivity of detection than HPLC method. Average contents of lignans in sesame germplasm evaluated in this study were 2.09~pm1.02mg/g of sesamin, and 1.65~pm0.61mg/g of sesamolin, respectively, showing significant variation for lignan components. The results showed that UV method for the determination of sesamin and sesamolin could be practically used as a faster and easier method than HPLC by using the regression equations developed in this study

Cyanidin 3-glucoside (C3G) content contained in the grains of blackish purple rice varieties, Heugjinjubyeo, Kilimheugmi, Heugnambyeo, Sanghaehy-anghyeolla, and the progenies derived from their crosses was evaluated by HPLC and UV-Vis spectroscopy. C3G content was higher in the range of 10-30% by using UV-Vis method compared to HPLC method. A significant linear relationship was, however, observed between two analytical methods. The correlation coefficient was 0.98. Thus, this results suggested that it would be able to use UV-Vis spectroscopy to determine C3G content which does not demanded precise value like selection.