• Journal of the Korean Society of Food Science and Nutrition
• /
• v.46 no.10
• /
• pp.1186-1194
• /
• 2017

Recently, many people have demanded reliable nutritional data even for minor-components. On the other hand, an analytical method for the analyses of vitamin $B_5$ and $B_6$ is lacking. Therefore, this study attempted to validate with accuracy and precision the analysis of vitamin $B_5$ and $B_6$ using a high-performance liquid chromatography (HPLC) method. The vitamin $B_5$ and $B_6$ contents were analyzed using an Agilent 1260 series HPLC system. YMC-Pack ODS-AM ($250{\times}4.6mm$ I.D.) and YMC-Pack Pro RS $C_{18}$ ($250{\times}4.6mm$ I.D.) columns were used for the analyses of vitamin $B_5$ and $B_6$, respectively. In the case of vitamin $B_5$, the flow rate was set to 1.0 mL/min by isocratic elution using the 50 mM $KH_2PO_4$ solution (pH 3.5)/acetonitrile (ACN) (95:5, v/v) with monitoring at 200 nm using HPLC/DAD, whereas the flow rate for vitamin $B_6$ was set to 1.0 mL/min of flow rate by isocratic elution using a 20 mM $CH_3CO_2Na$ solution (pH 3.6)/ACN (97:3, v/v) with monitoring by excitation at 290 nm and emission at 396 nm using HPLC/FLD. The column temperature was set to $30^{\circ}C$. The injection volume was $20{\mu}L$ for each experiment. The specificity of the accuracy and precision for vitamin $B_5$ and $B_6$ were also validated by HPLC. The results showed high linearity in the calibration curve for vitamin $B_5$ ($R^2=0.9998^{{\ast}{\ast}}$), the limit of detection (LOD) and limit of quantitation (LOQ) were 0.4 mg/L and 1.3 mg/L, respectively, In contrast, for the calibration curve of vitamin $B_6$, which showed high linearity ($R^2=0.9999^{{\ast}{\ast}}$), the LOD and LOQ were 0.006 mg/L and 0.02 mg/L, respectively.

• Korean Journal of Food Science and Technology
• /
• v.44 no.6
• /
• pp.686-691
• /
• 2012

The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.24 no.6
• /
• pp.848-858
• /
• 1995

The present study was conducted to investigate the effect of dietary vitamin A on the antioxidant status in ethanol-treated rats. Weaning rats were fed a basal diet until they reached about 160-180g body weight. Thereafter, four experimental groups were fed a liquid diet containing 36% ethanol of total calorie and four pair-fed groups were fed isocaloric sucorse instead of ethanol. Additionally, the liquid diet contained adequate amount of ${\beta}-carotene$, retinyl acetate, or 13-cis-retinoic acid except vitamin A deficient diet. The rats were sacrificed after 7 weeks of feedng periods. Significant decrease in hepatic vitamin E content was found in rats treated with chronic ethanol. However, dietary supplementation of retinyl acetate modified the change to some extent. Total vitamin C content of liver increased in vitamin A-deficient or ${\beta}-carotene$ groups with ethanol feeding. The ratio of reduced/oxidized vitamin C increased in the plasma and liver of ${\beta}-carotene$ group with ethanol feeding. Chronic ethanol intake did not change the total glutathione content of rat liver, but increased reduced glutathione(GSH)/oxidized glutathione(GSSG) ratio. This increase in hepatic GSH after chronic ethanol treatment. The changes of Se content in plasma and liver was not consistant. Fe content of liver increased by ethanol treatment, but this increase reduced in rats fed dietary retinyl acetate or 13-cis-retinoic acid. Fe content of plasma increased in vitamin A-deficient and ${\beta}-carotene$ supplemented groups with ethanol intake.

• Journal of Food Hygiene and Safety
• /
• v.19 no.1
• /
• pp.12-18
• /
• 2004

Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

• Journal of Embryo Transfer
• /
• v.19 no.1
• /
• pp.19-25
• /
• 2004

The objective of this study was to optimize the selection of sperm, optimal culture system of in vitro derived porcine embryos. The results obtained were summarized as follows: 1. When oocytes were inseminated with liquid sperm and frozen-thaw sperm, the cleavaged rate of liquid sperm (46.2%) was higher than that of frozen-thaw sperm (39.7%), however there were not show significant different each other. The blastocyst rates of liquid sperm (15.8%) was significantly higher than that of frozen-thawed sperm (9.3%)(P< 0.05). 2. When oocytes were inseminated with epididymal sperm after 1, 2 and 3 day storage, the cleavaged rate of epididymal sperm after 1, 2 and 3 day storage was 60.5, 61.0 and 56.8% respectively. The morulae (17.4, 19.9 or 17.3%) and blastocyst (8.7, 15.4, 11.3%) rate of epididymal sperm after 1, 2 and 3 day storage was no significantly respectively(P< 0.05). 3. In vitro developed to cleavaged rate of G1.3/G2.3 media used for culture was significantly(P< 0.05) higher as 62.1% compared with the results using the media NCSU23(52.8), however in vitro developed to blastocyst rate of NCSU23(11.6%) media was significantly(P< 0.05) higher than that'of G1.3/G2.3(4.7%). 4. When the fertilized oocytes were cultured with NCSU23 in addition to 1 mM glutathione(GSH), the cleavaged rate of treated groups of GSH(62.3%) was significantly higher than that of control(53.5%) respectively(P< 0.05). And in vitro developed to blastocyst rates of treated groups of GSH(15.6%) was higher than that of control(12.6%) however, there was no significant difference(P< 0.05).

• Journal of fish pathology
• /
• v.34 no.1
• /
• pp.71-80
• /
• 2021

Cephalexin, a semi-synthetic cephalosporin antibiotic, has long been used in fish aquaculture in various countries under legal authorization. The drug is thus widely available for use in other aquatic species except fishes like the crustacean whiteleg shrimp. This study aims to develop a sensitive method for laboratory residue studies to adopt in withdrawal period determinations. Through repeated trials from the existing methods developed for other food animal tissues, it was possible to achieve a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method. The results showed that at a concentration of 0.1 mg/kg, the recovery rate was 81.79%, and C.V. value was 8.2%, which meet the recovery rate and C.V. recommended by Codex guideline. After satisfactory validation of analytical procedures, applicability to the shrimp tissue was confirmed in experimentally cephalexin-treated whiteleg shrimp. As a result, most muscle samples were detected below the limit of quantification (0.05 mg/kg) after day 3, and most hepatopancreas samples were detected below the limit of quantification after day 14. In particular, the limit of quantification 0.05 ppm with the presently developed method suggests sufficient sensitive over the current legal maximum residue limit of 0.2 mg/kg set for fishes.

• The Korean Journal of Pesticide Science
• /
• v.17 no.4
• /
• pp.314-334
• /
• 2013

This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.46 no.8
• /
• pp.944-951
• /
• 2017

This study aimed to determine and examine the contents of vitamins $B_1$, $B_2$, and $B_3$ using the high-performance liquid chromatography method in traditional holiday foods in Korea. All analyses were under the quality control chart of vitamins $B_1$, $B_2$, and $B_3$. The z-scores for vitamins $B_1$, $B_2$, and $B_3$ were 1.3, 0.0, and 0.6, respectively, in food analysis performance assessment scheme proficiency tests assuring reliability of analytical performance. Vitamin $B_1$, $B_2$, and $B_3$ contents were analyzed in a total of 31 samples. Vitamin $B_1$, $B_2$, and $B_3$ contents ranged from 0.000 to 0.973 mg/100 g, from 0.037 to 0.264 mg/100 g, and from 0.000 to 1.223 mg/100 g in Korean traditional holiday foods, respectively. The highest contents of vitamins $B_1$, $B_2$, and $B_3$ were 0.973 mg/100 g in Yukwon-jeon, 0.264 mg/100 g in Dongtae-jeon, and 1.223 mg/100 g in Yukwon-jeon sample, respectively. However, compared to vitamins $B_2$ and $B_3$, vitamin $B_1$ was not detected, generally. Therefore, these results can be used as basic data for a food composition table and improvement of national health for Koreans.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.14 no.4
• /
• pp.365-369
• /
• 1985

In order to examine the effect of oil extraction methods on the characteristics of sesame oil, the unsaponifiable matters, fractionation sterol pattern and sterol compositions of the each fraction of the oil were compared in the oil extracted by the three different extraction methods, that is, pressure extraction of roasted seed (RTP), acetone extraction of roasted seed(RTE) and acetone extraction of raw seed(RWE). The amount of unsaponifiable in RWE oil was silghly higher as 31.8mg per 1mg drying oil than that in RTP oil of 26.1mg. Sesame oils from three different extraction methods were found to contain $0.26{\sim}0.32%$ free, $0.23{\sim}0.42%$ bound, and $0.49{\sim}0.64%$ total sterol. The content of free sterol in RWE oil was higher as 0.32% than that in RTE and RTP oil of 0.26%, and that of sterylglycoside in RTE oil was lower as 0.12% than that in RTP and RWE oil of 0.23%, but that of sterylester was a little difference. The unsaponifiable matter from fractionation sterol in sesame oil by three different extraction methods was fractionated into less polor compounds, 4,4-dimethyl-, 4-monomethyl-, 4-desmethylsterol fraction by thinlayer chromatography, and sterol composition of 4-desmethylsterol fraction was analyzed by gas liquid chromatography. The major sterols were campe-, stigma-, sito-, and ${\Delta}^5-avenasterol$, but, specially, unknown sterol(RRT:1.35) was found as $23.5{\sim}26.4%$ in total sterols, The content of sitosterol, ${\Delta}^5-avenasterol$, campesterol and stigmasterol were $59.9{\sim}60.3%,\;8.1{\sim}11%,\;16.1{\sim}18.4%,\;11.6{\sim}12.8%$ of the total sterol in free sterol fraction, $37.3{\sim}46.9,\;11.6{\sim}14.2,\;6.6{\sim}9.0$, and $6.1{\sim}8.0%$ of the total sterol in sterylglycoside fraction, $55.9{\sim}59.9,\;9.2{\sim}11.4,\;17.1{\sim}18.9$, and $11.8{\sim}13.7%$ of the total sterol in sterylester fraction, and $39.3{\sim}42.9,\;13.0{\sim}17.2,\;9.1{\sim}11.0$ and $7.4{\sim}11.5%$ of the total sterol in total sterol fraction. But the effect of oil extraction methods on sterol composition in sesame oil were hardly found.

• Korean Journal of Fisheries and Aquatic Sciences
• /
• v.19 no.4
• /
• pp.321-326
• /
• 1986

Oyster (Crassostrea gigas), arkshell (Anadare(Scapharce) broughtonii) and sea-mussel (Mytilus edulis) were investigated as to their lipid classes. Lipid extracts from shellfishes were fractionated into neutral lipid (NL), glycolipid (GL) and phospho-lipid (PL) by column chromatography with silicic acid. The fatty acid compositions of their lipid classes and lipid fractions were determined by gas liquid chromatography (GLC). Total lipid contents of shellfishes were $3.5\%$ in the oyster, $1.4\%$ in the arkshell, $1.0\%$ in the sea-mussel. The major fatty acids of total lipids were palmitic acid, eicosapentaenoic acid and docosahexaenoic acid in the oyster and the sea-mussel, palmitic acid, oleic acid and eicosapentaenoic acid in the arkshell. The lipid composition of neutral lipid fractions in shellfishes was separated and identified as free sterol, free fatty acid, triglyceride, hydrocarbon and esterified sterol by TLC. Of these classes, triglyceride fraction was most abundant, amounting to 55.6, 77.7 and $60.4\%$ in the three samples mentioned above, respectively. The main fatty acids of glycolipid were palmitic acid, eicosaenoic acid and docosahexaenoic acid in oyster, myristic acid, palmitic acid and palmitoleic acid in the arkshell, docosahexaenoic acid, linolenic acid and palmitic acid in the sea-mussel. The major fatty acids of phospholipid were palmitic acid, eicosapentaenoic acid and docosahexaenoic acid in the oyster and sea-mussel, palmitic acid, eicosapentaenoic acid and erucic acid in the arkshell.