Beauvericin과 enniatin H, I, 그리고 MK1688의 생산에 미치는 온도와 수분함량의 효과를 조사하였다. 쌀을 기질로 할 경우 25℃, 40% 수분함량에서 조사된 모든 독소들이 최대로 생산되었으며, 15℃의 온도에서 접종 2주 후 50 μg/g이하의 생성량을 나타내었다. 수분함량 10%에서도 접종 후 6주차에 모든 독소들의 검출이 확인되었으며, 이는 이 독소들이 0.75정도의 낮은 수분활성도에서도 생성될 수 있음을 나타낸다. 한편, 국내에서 생산된 곡류들(65종)에 대하여 Fusarium 독소인 beauvericin의 오염을 분석하였다. 국내에서 수확된 65종의 곡류시료 중 6종의 시료에서 beauvericin오염이 확인되었다. 쌀과 현미에서는 beauvericin이 검출되지 않았으며, 2004년산 옥수수 3종, 2004년과 2005산 보리 시료 각 1종, 그리고 2005년 재배된 밀 1종에서 beauvericin이 검출되었다. 가장 높은 오염도를 보인 것은 옥수수 시료이며, 이 시료에서 0.23 μg/g의 beauvericin이 검출되었다. 국내에서는 beauvericin에 대한 곡류 오염 조사가 이 연구에서 처음으로 이루어졌으며, 국내산 곡류에서도 beauvercin이 검출됨에 따라 지속적으로 오염도를 조사할 필요가 있다.

To resolve coelution phenomenon of acetone and acrolein in the HPLC‐based analysis of carbonyls, we attempted to find the optimal conditions for their separation. For the purpose of this study, the collection of carbonyl Compounds is made by DNPH‐coated cartridges. Quantification of carbonyls is then initiated by the formation of hydrazone derivatives that are then separated by HPLC and detected by UV‐VIS spectroscopic detector (at 360 nm). To the course of this experiment, we examined the influences of the three major experimental variables such as 5 temperature (25, 30, 40, 50 and 60℃), 2 flow rate (1.0 and 1.2 mL min‐1), and variable relative composition of mobile phase (among acetonitrile, water, and tetrahydrofuran). According to our experiments, the optimal condition for separation was found at flow rate of 1.2 mL min‐1 and temperature of 32℃ with the mobile phase composition of acetonitrile:water:tetrahydrofuran = 34 : 52.8 : 13.2.

On the analysis of triacylglycerol (TG) from the kernels of Acanthopanax sessiliflorus by reversed phase-HPLC, it was separated into three main fractions of PN 44, 46 and 48, according to partition number (PN). On the contrary, it could be clearly classified into seven fractions of SMM, MMM, SMD, MMD, SDD, MDD and MDT by silver ion-HPLC by the number of double bond in the acyl chains of TG species. But resolution of so-called critical pairs of TG molecular species such as molecular pairs of PeLL [C18:1Ω12/(C18:2Ω6)2] and OLL [C18:1Ω9/(C18:2Ω6)2] and OOL [(C18:1Ω9)2/C18:2Ω6], and PePeL [(C18:2Ω12)2/C18:1Ω6] was not achieved (Pe; petroselinic acid, L; linoleic acid, O; oleic acid). On the other hand, TG extracted from Aralia continentalis kernels were also fractionated into seven groups of SSM, SMM, MMM, SMD, MMD, SDD and MDD (S; saturated acid, M; monoenoic acid, D; dienoic acid) by silver ion-HPLC, although it's were classified into three groups of PN 44, 46 and 48 by reversed phase-HPLC. The fractions of SMM, MMM, MMD and MDD were divided into two subfractions, respectively; the fractions of SMM, MMM, MMD and MDD were resolved into the subfraction of PPe/Pe and POO (critical pairs from each other), that of Pe/Pe/Pe and OOO, that of Pe/Pe/L and OOL, and that of Pe/L/L and OLL.

1. 닭고기에서 4종의 플루오로퀴놀론계 합성항균제(ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin)를 액상추출법으로 추출하여 형광검출기와 HPLC를 이용하여 동시 정량분석하는 방법을 확립하였으며 분석조건으로서 컬럼은 Symmetry C18(250×4.6 mm id, 5 ㎛), 이동상은 0.4% triethylamine 및 0.4% phospholic acid 수용액, methanol 및 acetonitrile 혼합용액(800:100:100, v/v/v)을 사용하였으며, 형광검출기는 여기파장 278 nm, 측정파장 456 nm으로 그리고 유속은 1.0 ml/min., 주입량은 50 ㎕로 하였다. 확립된 분석조건으로 측정한 ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin 표준품의 표준곡선식에서 모두 상관계수 0.999이상의 양호한 직선성을 보였으며, 첨가한 닭고기의 크로마토그람에서도 각각의 nfwlfquf 분리시간대에 방해 피크 없이 양호한 분리도를 나타내었다. 0.05~0.2 ㎍/g 첨가한 시료에서 평균 회수율은 ofloxacin 92.0~95.4%, norfloxacin 84.2~87.3%, ciprofloxacin 78.3~82.2%, enrofloxacin 91.3~95.3%이었으며 변이계수(CV)는 2.7~9.4%이었다.4종의 동시분석법의 검출한계 및 정량한계는 각각 ofloxacin 23.5 ppb, 35.3 ppb, norfloxacin 3.4 ppb, 5.1 ppb, ciprofloxacin 3.0 ppb, 4.5 ppb, enrofloxacin 2.5 ppb, 3.8 ppb 수준이었다. 2. 인천 지역에서 돛구한 닭고기 총 1,523수를 EEC-4-plate법으로 검사한 결과 양성반응을 보인 닭고기는 15수(육계 10, 토종닭 5)였으며, HPLC를 이용한 정밀검사결과 육계 5수에서 ciprofloxacin이 불검출~0.04 ppm, enrofloxacin이 0.01~0.69 ppm수준으로 검출되었으며, 토종닭 5수에서는 ciprofloxacin이 0.02~0.12 ppm, enrofloxacin이 0.36~6.79 ppm수준으로 검출되었다.

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,,, 40 pm, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, C,,/egg and Na2S0, matrix were transferred to a column made of 10 ml glass synnge and filter paper and compressed 4.0-4.5 ml volume. The column was washed with 8 ml of hexane and dried under N, 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 ngig of eggs, 20 pl 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.

Conjugate trienoic acids (CTA) occurred in triacylglycerols (TGs) of the seed oils of Trichosanthes kirilowii, Momordica charantia and Aleurites fordii, and they were easily converted to their methyl esters in a mixture of sodium methoxide-methanol without any structural destruction. The main fatty acids in triacylglycerol (TG) fraction of the seed oils of Trichosanthes kirilowii are C18:2Ω6 (32.2 mol %), C18:3 9c.11t,13c (38.0 mol %) and C18:1Ω9 (11.8 mol %), followed with C16:0 (4.8 mol %) and C18:0 (3.1 mol %). The TG fraction was resolved into 20 TG molecular species according to the partition number (PN) by reversed-phase (RP)-HPLC. The main TG species were DTc2, MDTc and D2Tc, of which amounts reached 63 mol % of total TG molecular species. The TG sample was fractionated into 11 fractions according to the number of double bond in the molecule by Ag+-HPLC and the species of DTc2, MDTc and D2Tc were also eluted as main components. The TG species containing CTA showed unusual behaviours in the order of elution by HPLC ; first, TG moleular species of DTc2 (D; dienoic acid, Tc; punicic acid, Tci; α-eleostearic acid, M ; monoenoic acid, St; stearic acid) was eluted earlier than Mtc2, although they have the same PN number of 40, and, secondly, the species of DTci2 with eight double bonds was eluted earlier than that of D2Tci with seven double bonds. Intact TG of the seed oils of Momordica charantia contained mainly fatty acids such as C18:3Ω9c,11t,13t (57.7 mol %), C18:1Ω9 (17.4 mol %), C18:0 (12.3 mol %) and C18:2Ω6 (10.6 mol %), and was classified into 13 fractions by RP-HPLC. The main TG species were as follows ; MTci2 [(C18:1Ω9)(C18:3 9c,11t,13t)2, 39.1 mol %] and StTci2 [(C18:0)(C18:3 9c,11t,13t)2, 33.9 mol %] comprising about 73 mol % of total TG species, accompanied by DTci2 [(C18:2Ω6)(C18:3 9c,11t,13t)2, 7.3 mol %], D2Tci [ (C18:2Ω6)2(C18:3 9c,11t,13t), 3.6 mol %] and MDTci [(C18:1Ω9)(C18:2Ω6)(C18:3 9c,11t,13t), 3.5 mol %]. Simple TG species of Tci3 [(C18:3 9c,11t,13t)3] was present in a small amount of 1.4 mol %, but other simple TG species were not detected. The TG was also resolved into 11 fractions according to the number of double bond by Ag+-HPLC, and the species were mainly occupied by MTci2 [(C18:1Ω9)(C18:3 9c,11t,13t)2, 39.4 mol %] and StT-ci2 [(C18:0)(C18:3 9c,11t,13t)2, 35.4 mol %] DTci2 species with eight double bonds was also developed faster than D2Tci one with seven double bonds as indicated in the analysis of TG of the seed oils of T. kirilowii, and MTci2 species with cis, trans, trans-configurated double bond was eluted earlier than MTc2 species with cis, trans, cis-configurated double bond. The main components of fatty acid in total TG fraction isolated from the seed oils of of Aleurites fordii were in the following order ; C18:3 9c,11t,13t (81.2 mol %)〉 C18:2Ω6 (8.5 mol %)〉 C18:1Ω9 (5.4 mol %). With resolution of the TG by RP-HPLC, eight fractions such as Tci3, Dtci2, D2Tci, MTci2, PTci2 (P; palmi..