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

• Bulletin of the Korean Chemical Society
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• v.24 no.5
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• pp.559-565
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• 2003

An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.195-201
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• 2012

We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

• Journal of Food Hygiene and Safety
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• v.22 no.2
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• pp.88-92
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• 2007

Isopropylthioxanthone(ITX) is used as a photoinitiator In UV-cured inks, triggering the radical polymerization of the acrylic component of such inks and thus causing the liquid ink film to cure. Recently ITX was detected in carton packed food in Italy. In order to cope with risk issues of overseas and acquire monitoring data on ITX, we have established the method using HPLC/FLD for ITX analysis after reviewing parameters of the analytical methods. Limit of detection (LOD) and limit of quantification (LOQ) were 0.02 ppb and 0.1 ppb, and linearity and RSD (%) were 0.9991 and 1.09, respectively. We have investigated ITX levels migrated to food on 87 commercial products packed in carton and ITX was not detected any food. Therefore it is supposed that UV-cured ink containing ITX as photoinitiator is not currently used in printing of carton pack in Korea.

• Korean Journal of Food Science and Technology
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• v.42 no.5
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• pp.632-636
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• 2010

The level of ${\gamma}$-aminobutyric acid (GABA) in pigmented rice was quantitatively and qualitatively determined by high pressure liquid chromatography/fluorescence detection (HPLC/FLD). In this study, the recovery rate and limit of detection (LOD) of GABA were 122.4${\pm}$2.4% and 0.23 ${\mu}g/g$, respectively. The geminating pigmented rice samples, which were harvested in Paju, Korea, were soaked in water at $18^{\circ}C$ for 20 hr. After soaking, the samples were germinated at $30^{\circ}C$ for about 24 hr. GABA content was highest (293.0 ${\mu}g/g$) in the germinated red rice. Furthermore, GABA levels in the germinated rice increased significantly by up to 11.1 and 24.7-fold as compared to non-germinated rice and milled rice, respectively. The GABA concentrations of non-germinated rice, with the exception of red rice, were significantly higher than those of milled rice by 7.6-20.6-fold.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.441-452
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• 2011

This study was carried out to survey the residual characteristics of endocrine disruptor (ED)-suspected pesticides in greenhouse soils and assess their leachabilites to groundwater. Greenhouse soils were collected from 40 sites of greenhouse in 2008 in Korea. Sixteen ED-suspected pesticides which had been using in Korea, such as alachlor, benomyl, carbaryl, cypermethrin, 2,4-D, dicofol, endosulfan, fenvalerate, malathion, mancozeb, metribuzin, metiram, methomyl, parathion, trifluralin, and vinclozolin, in the soils, were analyzed by chromatographic methods using GLC-ECD and HPLC-DAD/FLD. Limits of detection (LODs) of the test pesticides ranged from 0.0004 to 0.005 mg/kg. Recoveries of the target pesticides from soil ranged from 72.69 to 115.28%. Four pesticides including cypermethrin were detected in the range of from 0.001 to 2.019 mg/kg, representing that their detection rate from greenhouse soils was 37.5%. The highest detection rate was observed from endosulfan which was detected from 16 site soils of the total samples, indicating that endosulfan is persistent in soil because of its very low mobility and high adsorption characteristics in soil. Based on the groundwater ubiquity scores (GUSs) of the pesticides detected from greenhouse soils, most of them have little possibilities of groundwater contamination except the fungicide vinclozolin with some leaching potential because of high water solubility and very low soil adsorption property.

• Journal of Food Hygiene and Safety
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• v.26 no.3
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• pp.214-221
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• 2011

Deoxynivalenol (DON) and zearalenone (ZEN) are mainly contaminated mycotoxins in feeds. The study was carried out to analyze and survey the contamination of DON and ZEN in one hundred thirteen samples of feeds. After cleaning all samples with immunoaffinity column, the mycotoxins were analysed by using high performance liquid chromatography/fluorescence with diode array detector (HPLC/FLD with DAD). The average recoveries of DON were 88.76 and 95.40% at the levels of 200 and 1,000 ${\mu}g/kg$ and 87.09 and 98.40% of ZEN were recovered at the levels of 100 and 500 ${\mu}g/kg$, respectively. The limit of detection (LOD) were 6.0 and 3.0 ${\mu}g/kg$ for DON and ZEN, respectively. The average concentrations of DON were 372.1, 324.0 and 990.9 ${\mu}g/kg$ in chicken, pig and cattle feed, respectively. Those of ZEN were 76.1, 43.7 and 196.2 ${\mu}g/kg$ for them, individually.

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.308-314
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• 2012

In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

• Food Science of Animal Resources
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• v.41 no.4
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• pp.731-738
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• 2021

Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.

• Journal of Food Hygiene and Safety
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• v.33 no.5
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• pp.339-346
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• 2018

This study was conducted to monitor the current status of pesticide residues in a total of 297 agricultural products for raw juice from January 2017 to September 2017. Pesticide residues in samples were analyzed by multiresidue method for the determination of multiclass pesticide with an aim to detect 220 pesticides using GC/ECD, GC/NPD, TOF/MS, LC/PDA, LC/FLD, and LC/MS-MS. The analysis revealed the presence of nine pesticides in 14 samples. The detected pesticides were chlorpyrifos, cyflufenamid, chlorothalonil, pendimethalin, azoxystrobin, pyridalyl, imazalil, fludioxonil and procymidone. The kinds of detected crops were mandarin, carrot, apple, celery, chicory, orange and grape. Risk assessment evaluated human health exposure with the ratio of EDI (Estimated daily intake) to ADI (Acceptable daily intake) of pesticides detected and the range of %ADI (the ratio of EDI to ADI) values was 0.0011~6.7087% and safety level.