• Analytical Science and Technology
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• v.25 no.4
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• pp.257-264
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• 2012

Penicillins belong to the ${\beta}$-lactam class of antibiotics, and are frequently used in human and veterinary medicine. Despite the positive effects of these drugs, improper use of penicillins poses a potential health risk to consumers. This study has been undertaken to determinate multi-residues of penicillins, including amoxicillin, ampicillin, oxacillin, bezylpenicillin, cloxacillin, dicloxacillin, and nafcillin, using liquid chromatographic tandem mass spectrometer (LC-MS/MS). The developed method was validated for specificity, precision, recovery, and linearity in livestock and marine products. The analytes were extracted with 80% acetonitrile and clean-up by a single reversed-phase solid-phase extraction step. Six penicillins presented recoveries higher than 76% with the exception of Amoxicillin. Relative standard deviations (RSDs) were not more than 10%. The method was applied to 225 real samples. Benzylpenicillin was detected in 12 livestock products and 7 marine products. Amoxicillin, ampicillin, cloxacilllin, dicloxacillin, nafcillin and oxacillin were not detected. The detected levels were 0.001~0.009 mg/kg in livestock products excluding eggs and milk. In marine products, the detected levels were under 0.03 mg/kg. They were under the MRL levels. As monitoring results, it is identified to be safe but it is considered that safety management of antibiotics should continue by monitoring.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.202-208
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• 2012

A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.372-379
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• 2007

A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

• Korean Journal of Food Science and Technology
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• v.36 no.6
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• pp.893-899
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• 2004

Method for sample preparation and quantitative analysis of 19 permitted and non-permitted synthetic colors in foods was developed based on reversed-phase ion-pairing high performance liquid chromatography. For color extraction of samples, deionized water was added, and pH was appropriately adjusted with 1% ammonia water. Any undissolved matters were extracted with 50% ethanol or 70% methanol. Lipid in snacks was first removed using n-hexane with centrifugation, water was added to extract colors, followed by clean-up and concentration using Sep-Pak $C_{18}$ cartridge. Recovery efficiencies at known concentrations of 19 standard food colors spiked into foods were in 90.3-97.9% range far soft drink, 79.2-101.9% for candy, 84.1-103.4% for jelly, 86.4-100.8% for chewing gum, 83.5-103.4% for ice cream, and 78.5-95.6% for snack.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.381-388
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• 2017

In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.329-335
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• 2017

Analysis method was presented for the simultaneous determination of nine bisphenol A related compounds such as bisphenol A (BPA), phenol, p-tert-butylphenol, bisphenol A diglycidyl ether (BADGE), $BADGE{\cdot}2H_2O$, $BADGE{\cdot}2HCl$, bisphenol F diglycidyl ether (BFDGE), $BFDGE{\cdot}2H_2O$ and $BFDGE{\cdot}2HCl$ migrated from inner coatings of metal food cans by high performance liquid chromatography (HPLC) with fluorescence detection. The method was validated by examining the linearity of calibration curve, the limit of detection (LOD), the limit of quantification (LOQ), recovery and uncertainty. The migration tests of nine BPA related compounds were carried out with four food simulants; deionized water (DW), 4% acetic acid, 50% ethanol and n-heptane. There was not any compound detected in DW, 4% acetic acid and 50% ethanol at $60^{\circ}C$ for 30 min and n-heptane at $25^{\circ}C$ for 60 min. BPA and phenol were migrated into 4% acetic acid and 50% ethanol at $95^{\circ}C$ for 30 min. The concentrations were ranged from 0 to $10.77{\mu}g/L$ of BPA and from 0 to $2.35{\mu}g/L$ of phenol. Canned foodstuffs mostly have long-term shelf life. We investigated migration of nine BPA related compounds according to the variation in storage periods (0~90 days) and temperatures (4, 25 and $60^{\circ}C$). All compounds were not founded during 90 days at $4^{\circ}C$ and $25^{\circ}C$, respectively. However BPA and $BADGE{\cdot}2H_2O$ were founded in DW and 4% acetic acid at $60^{\circ}C$. The migration levels of BPA and $BADGE{\cdot}2H_2O$ were close to the value of LOQ, respectively and did not change significantly as storage period. It was founded from results that the migration of BPA related compounds from metal food cans was controlled to a safe level.

• Korean Journal of Food Science and Technology
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• v.45 no.4
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• pp.391-402
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• 2013

Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.

• Korean Journal of Food Science and Technology
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• v.45 no.1
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• pp.111-119
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• 2013

Eleven mycotoxins, including aflatoxins, ochratoxin A, fumonisins, zearalenone, T-2 toxin, deoxynivalenol, and HT-2 toxin, were analyzed simultaneously in rice, barley, and maize produced in 2011 by liquid chromatography coupled with triple quadrupole mass spectrometry (LC/MS/MS). Limits of detection (LOD) are 0.2 ${\mu}g/kg$ for aflatoxin $B_1$, and $G_1$, 0.3 ${\mu}g/kg$ for aflatoxins $B_2$, and $G_2$, 0.1 ${\mu}g/kg$ for ochratoxin, fumonisins, zearalenone, and T-2 toxin and 3.0 ${\mu}g/kg$ for deoxynivalenol and HT-2 toxin. Limits of quantification (LOQ) were 0.6 ${\mu}g/kg$ for aflatoxins $B_1$, and $G_1$, 0.9 ${\mu}g/kg$ for aflatoxins $B_2$, and $G_2$, 0.3 ${\mu}g/kg$ for ochratoxin, fumonisins, zearalenone, and T-2 toxin and 10.0 ${\mu}g/kg$ for deoxynivalenol and HT-2 toxin. Recoveries for 11 mycotoxins ranged from 70.45 to 111.11%. Fumonisins, deoxynivalenol, and zaeralenone were detected from 0.9 to 334.0 ${\mu}g/kg$ in the polished rice, barley and raw corn cultivated in Korea. Other mycotoxins were not detected. Deoxynivalenol contamination was mainly found in barley (24 out of 43 samples) and the average value in positive samples was 113.30 ${\mu}g/kg$.

• Korean Journal of Food Science and Technology
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• v.40 no.2
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• pp.152-159
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• 2008

The purpose of this study was to determine the accurate quantification of vitamin A in infant formula by comparing two different standard stock solutions as well as various sample weights using high performance liquid chromatography. The sources of uncertainty in measurement, such as sample weight, final smaple vloume, and the instrumental results, were identified and used as parameters to determine the combined standard uncertainty based on GUM(guide to the expression of uncertainty in measurement) and the Draft EURACHEM/CITAC Guide. The uncertainty components in measuring were identified as standard weight, purity, molecular weight, dilution of the standard solution, calibration curve, recovery, reproducibility, sample weight, and final sample volume. Each uncertainty component was evaluated for type A and type B and included to calculate the combined uncertainty. The analytical results and combined standard uncertainties of vitamin A according to the two different methods of stock solution preparation were 627 ${\pm}$ 33 ${\mu}$g R.E./100 g for 1,000 mg/L of stock solution, and 627 ${\pm}$ 49 ${\mu}$g R.E./100 g for 100 mg/L of stock solution. The analytical results and combined standard uncertainties of vitamin A according to the various sample weighs were 622 ${\pm}$ 48 ${\mu}$g R.E./100 g, 627 ${\pm}$ 33 ${\mu}$g R.E./100 g, and 491 ${\pm}$ 23 ${\mu}$g R.E./100 g for 1 g, 2 g, and 5 g of sampling, respectively. These data indicate that the preparation method of standard stock solution and the smaple amount were main sources of uncertainty in the analysis results for vitamin A. Preparing 1,000 mg/L of stock solution for standard material sampling rather than 100 mg, and sampling not more than 2 g of infant formula, would be effective for reducing differences in the results as well as uncertainty.

• Horticultural Science & Technology
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• v.34 no.1
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• pp.172-182
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• 2016

This study was aimed to determine the changes in vitamin $B_5$ and $B_6$ contents compared to fresh materials after parboiling treatment of the main vegetables consumed in Korea. The specificity of accuracy and precision for vitamin $B_5$ and $B_6$ analysis method were validated using high-performance liquid chromatography (HPLC). The recovery rate of standard reference material (SRM) was excellent, and all analysis was under the control line based on the quality control chart for vitamin $B_5$ and $B_6$. The Z-score for vitamin $B_6$ in food analysis performance assessment scheme (FAPAS) proficiency test was -1.0, confirming reliability of analytical performance. The vitamin $B_5$ and $B_6$ contents in a total of 39 fresh materials and parboiled samples were analyzed. The contents of vitamin $B_5$ and $B_6$ ranged from 0.000 to 2.462 and from 0.000 to $0.127mg{\cdot}100g^{-1}$, respectively. The highest contents of vitamin $B_5$ and $B_6$ were $2.462mg{\cdot}100g^{-1}$ in fresh fatsia shoots (stem vegetables), and $0.127mg{\cdot}100g^{-1}$ in fresh spinach beet (leafy vegetables), respectively. Moreover, the vitamin $B_5$ and $B_6$ contents for parboiling treatment in most vegetables were reduced or not detected. In particular, the contents of vitamin $B_5$ in parboiled fatsia shoots and vitamin $B_6$ in parboiled yellow potato and spinach beet were decreased 20- and 4-fold compared with fresh material, respectively. These results can be used as important basic data for utilization and processing of various vegetable crops, information for dietary life, management of school meals, and national health for Koreans.