• 한국식품위생안전성학회지
• /
• 제13권1호
• /
• pp.41-46
• /
• 1998

HPLCdp 의한 주요 afltoxins(aflatoxins $B_1,\;B_2,\;G_1\;및\;G_2$)의 동시 분석에서 postcolumn 유도체화법을 시도하였다. Electrochemical cell (Kobra-cell)을 사용한 postcolumn 유도체화법은 기존의 precolumn 유도체화법보다 분석시간을 단축하였으며 (약 1/2 단축), 더 안전하고 , 향상된 분석능을 보였다. Aflatoxin $B_1과\;G_1의$ 경우 10~100ppb에서, 그리고 B_2와\;G_2의$ 경우 3~30 ppb에서 직선성을 나타내었다. Aflatoxin $B_1과\;G_1은$ 각각 88.9% 및 100.5%로 양호한 회수율을 보였다. Aflatoxin $B_2와\;G_2의$ 경우 분리도는 우수하였으나 회수율에있어서 변이가 크게 나타났다.

• Bulletin of the Korean Chemical Society
• /
• 제34권6호
• /
• pp.1783-1790
• /
• 2013

A simultaneous analytical method has been developed for the fluorimetric determination of haloacetonitriles (HANs) [dichloroacetonitrile (DCAN), trichloroacetonitrile (TCAN), dibromoacetonitrile (DBAN), haloacetamides [dichloroacetamide (DCAD), and trichloroacetamde (TCAD)] in drinking water by using the combined on-line perconcentration/reversed phase liquid chromatography (RPLC)-postcolumn detection system. This on-line perconcentration system was achieved by employing a precolumn packed with a commercial solid phase extraction (SPE) sorbent for the enrichment and purification of the target analytes. The haloacetonitriles and haloacetamides were separated on CN analytical column in a 7.5% methanol-0.02 M phosphate buffered mobile phase at pH 3. The column effluents were reacted with postcolumn reagents of ophthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which were measured with a fluorescence detector. Under the optimized conditions for RPLC and the postcolumn derivatization system all of the coefficient of determination of the standard calibration curves for the target analytes were over 0.99 and had a linear range from 5 to 100 ${\mu}g/L$. The detection limits showed 1.6 ${\mu}g/L$ for DCAD, 0.1 ${\mu}g/L$ for TCAD, 0.6 ${\mu}g/L$ for DCAN, 1.6 ${\mu}g/L$ for TCAN and 1 ${\mu}g/L$ for DBAN, and the recoveries were ranged from 64 to 99% except for DCAD with precisions less than 4.9% in distilled water, and from 72(${\pm}4%$) to 116%(${\pm}2%$) in tap water.

• 한국식품위생안전성학회지
• /
• 제11권2호
• /
• pp.149-157
• /
• 1996

A procedure for the determination of Aflatoxins in food and grains which utilizes reversed phased liquid chromatographic (LC) analysis with postcolumn derivatization by an electrochemical cell and determination with a fluorescence detector has been evaluated. The LC mobile phase was water-acetonitrile-methanol (6+2+2) with 1mM KBr and 1 mM HNO3 which gave baseline separation for the four Aflatoxins (AfB1, AfB2, AfG1, AfG2). The electrochemical cell set at 7V, generated bromine and derivatized aflatoxins B1 and G1, The derivatives were detected by the fluorescence detector. The aflatoxins in naturally contaminated corn samples were isolated by three different cleanup procedures: the AOAC method I column(CB method), a rapid filtrate column (Romer's column), and an immunoaffinity column. The final extract were quantitated with fluordensitometric TLC and the LC postcolumn derivatization techniques. The results were quite similar, however the LC technique showed less interferences and could be automated. Samples of corn, raw peanuts, peanut butter and dried dates were also analyzed successfully with this procedure.

• Bulletin of the Korean Chemical Society
• /
• 제25권6호
• /
• pp.900-906
• /
• 2004

An RPLC-postcolumn detection method has been developed for the fluorimetric determination of dichloroacetamide (DCAD) in water. After ammonia and DCAD were separated on a $C_{18}$ nonpolar stationary phase with 2.5% methanol-0.02 M phosphate buffer at pH 3, the column eluant was reacted with post column reagents, o-phthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which was measured with a fluorescence detector ( ${\lambda}_{ex}$ = 363 nm, ${\lambda}_{em}$ = 425 nm). With the optimized conditions for RPLC and the postcolumn derivatization, the calibration curve was found to be linear in the concentration ranges of 0.5 and 20 ${\mu}$M for DCAD, and the detection limit for DCAD was 0.18 ${\mu}$M (23${\mu}$g/L). This corresponded to 18 pmol per 100 ${\mu}$L injection volume for a signal-to-noise ratio of 3, and the repeatability and reproducibility of this method were 1.0% and 2.5% for five replicate analyzes of 2 ${\mu}$M DCAD, respectively. The degradation yields DCAD to ammonia were 94 and 99%, and the percent recoveries of DCAD from 4 and 6 ${\mu}$M DCAD-spiked tap water were shown mean more than 97%.

• 한국대기환경학회지
• /
• 제22권3호
• /
• pp.297-307
• /
• 2006

During January $2002{\sim}April\;2004$, hydrogen peroxide ($H_{2}O_{2}$) measurements were performed at the campus of Korea University, which is located in the northeastern part of Seoul. Gas phase hydroperoxide was collected in aqueous solution and separated by HPLC. Concentrations were determined by fluorescence using postcolumn enzyme derivatization. This measurement system was improved to be run automatically from sample collection at every 10 minutes through chemical analysis for data collection. Detection limits of $H_{2}O_{2}$ is $10{\sim}17\;pptv$, and the overall uncertainty of the measurements is better than 8%. Two-year measurements of $H_{2}O_{2}$ show typical seasonal variations. Concentrations of $H_{2}O_{2}$ were higher during $June{\sim}October$ and lower during $January{\sim}February$. Maximum concentration of 1-hour averaged $H_{2}O_{2}$ was 6.5 ppbv, which was observed in August and September. In general $H_{2}O_{2}$ concentrations were well correlated with $O_{3}$ concentrations and largely affected by meteorological factors such as temperature and wind direction.

• 한국대기환경학회지
• /
• 제21권6호
• /
• pp.689-697
• /
• 2005

Hydrogen peroxide is a reservoir of OH radical which is the powerful oxidant in the atmosphere. Therefore, the status of the oxidizing atmosphere could be reflected on the concentration of $H_{2}O_{2}$. In this study, the distribution of $H_{2}O_{2}$ was determined during the intensive aircraft measurements over the Yellow sea in March, December 2002, April, November 2003 and March, October 2004. Flights covered from $124^{circ}E\;to\;129^{circ}E\;and\;35^{circ}N\;to\;37^{circ}N$, and extending to 3,000 m. The flight patterns were set properly to assess the altitudinal and longitudinal distribution for $H_{2}O_{2}$. $H_{2}O_{2}$ was extracted onto aqueous solution using a continuously flowing glass coil and analyzed by a high performance liquid chromatography (HPLC) accompanied with a fluorescence detector using postcolumn enzyme derivatization. Mixing ratios of $O_{3},\;NO_{x}\;and\;SO_{2}$ were measured in real time by commercial analysis instruments. Along the heights, the maximum concentration of $H_{2}O_{2}$ appeared around 1,500 m then gradually decreased with increasing altitude. The vertical behavior of ozone showed the similar trend to $H_{2}O_{2}$. The mean mixing ratio of $NO_{x}$ was about 2 ppbv and not showed clear vertical distribution patterns. The mean value of was the same as $NO_{x}$ however $SO_{2}$ appeared extreme concentration in low altitude. $H_{2}O_{2}\;and\;O_{3}$ showed even longitudinal distribution however $NO_{x}$ mixing ratio in land ($127^{circ}E$) was much higher than over the sea. $SO_{2}$ rather decreased with increasing longitude. $H_{2}O_{2}$ was in inverse proportion to $NO_{x}$ in spring and summer and $SO_{2}$ in spring, which indicated its significant role to NO and $SO_{2}$ oxidation pathways.