• Analytical Science and Technology
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• v.20 no.2
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• pp.138-146
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• 2007

A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

• Analytical Science and Technology
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• v.21 no.6
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• pp.518-525
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• 2008

Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

• Food Science and Preservation
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• v.20 no.6
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• pp.877-885
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• 2013

Wine extracts of four different berry fruits, such as mulberry, blueberry, strawberry, and raspberry, were investigated for antioxidant, anti-tyrosinase, and ${\alpha}$-glucosidase activities by using in vitro assays. Additionally, quantitative changes of ${\alpha}$-glucosidase inhibitor in mulberry wine were determined by HPLC according to mulberry cultivars and fermentation process. Among four berry wines examined, mulberry wine showed the most potent ${\alpha}$-glucosidase inhibitory activity with 69.37% at 0.23 mg/mL, while blueberry and strawberry wines exhibited the strongest inhibition against DPPH radical and tyrosinase activity, respectively. Four compounds were isolated and purified from mulberry wine by a series of isolation procedures, such as solvent fractionation, and Diaion HP-20, ODS-A, and Sephadex LH-20 column chromatographies. Among them, Comp. 4 exerted the strongest ${\alpha}$-glucosidase inhibitory activity ($I_C_{50}=31.57{\mu}M$), and its chemical structure was identified as quercetin by UV and NMR spectral analysis. Finally, the "Daeseongppong" (16.83 ppm) muberry wine had larger amount of quercetin than the "Iksuppong" (14.85 ppm) and "Cheongilppong" (8.92 ppm) mulberry wines, but their contents of three mulberry wines decreased considerably with aging process. These results suggest that mulberry wine containing quercetin acted as ${\alpha}$-glucosidase inhibitor may be useful as a potential functional wine for improving diabetic disorder.

• Journal of the Korean Society of Food Science and Nutrition
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• v.40 no.4
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• pp.517-524
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• 2011

Eleven polyphenolic compounds, including procatechuic and chlorogenic acids, (+)-dihydroquercetin, rutin, isoquercitrin, quercitrin, (+)-dihydrokaempferol, trans-resveratrol, moracin, quercetin and 4-prenylmoracin were isolated and purified from the methanolic extract of defatted mulberry seed residue by a series of column chromatography including silica gel, Sephadex LH-20, and ODS-A, and their chemical structures were identified by spectral analysis. The antioxidant activities of the eleven isolated polyphenolic compounds were measured spectrophotometrically using DPPH radical. Among the eleven polyphenolic compounds tested, rutin ($IC_{50}=20.2\;{\mu}M$), isoquercitrin ($IC_{50}=22.5\;{\mu}M$), quercitrin ($IC_{50}=24.6\;{\mu}M$), quercetin ($IC_{50}=27.8\;{\mu}M$), (+)-dihydroquercetin ($IC_{50}=28.9\;{\mu}M$), and chlorogenic acid ($IC_{50}=30.6\;{\mu}M$) exhibited stronger antioxidant activity than L-ascorbic acid ($IC_{50}=31.5\;{\mu}M$) and ${\alpha}$-tocopherol ($IC_{50}=52.3\;{\mu}M$), whereas procatechuic acid ($IC_{50}=68.2\;{\mu}M$) showed lower activity. In addition, (+)-dihydrokaempferol ($IC_{50}=33.8\;{\mu}M$), trans-resveratrol ($IC_{50}=36.2\;{\mu}M$), moracin ($IC_{50}=47.6\;{\mu}M$), and 4-prenylmoracin ($IC_{50}=48.2\;{\mu}M$) exhibited moderate antioxidant activity. Furthermore, levels of the eleven polyphenolic compounds from three different types of mulberry seeds were quantified by HPLC, and their contents were as follows: rutin (311~60.0 mg/100 g)> quercitrin (7.2~34.2 mg/100 g)> (+)-dihydroquercetin (13.2~33.1 mg/100 g)> quercetin (15.8~19.5 mg/100 g)> 4-prenylmoracin (10.5~43.3 mg/100 g)> isoquercitrin (5.8~15.4 mg/100 g)> chlorogenic acid (0.0~15.3 mg/100 g)> moracin (4.7~7.2 mg/100 g)> procatechuic acid (0.0~11.6 mg/100 g)> (+)-dihydrokaempferol and trans-resveratrol (<0.1 mg/100 g). The 'Daesungppong' mulberry seeds among the three cultivars had higher flavonoid contents, such as rutin and quercetin derivatives, while the 'Iksuppong' seeds had the highest contents of phenolic acids and moracin derivatives. 'Cheongilppong' had lower amounts of polyphenolic compounds than the other two mulberry seeds. These results indicate that mulberry seeds containing antioxidant polyphenolic compounds may be potentially useful sources of anti-diabetic, anti-hypertensive, and anti-aging agents for functional foods and cosmetics.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.413-420
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• 2019

In this study, a sample preparation method and a simultaneous determination method by ultra-high performance liquid chromatography coupled with tandem mass spectrometry for 9 isomers of chlorogenic acid and arbutin in fruits were developed. The samples were extracted using 90% methanol (pH 3.0), with the solutions being shaken and then sonicated for 10 min each. After centrifugation at 4,000 rpm for 10 min, the extraction was concentrated under a vacuum at $40^{\circ}C$ using a vacuum evaporator. The residue was dissolved in 5 mL of 5% methanol and filtered through a $0.45{\mu}m$ membrane before UHPLC-MS/MS analysis. The separations were performed on a C18 column with gradient elution of water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid). The specificity, linearity, limit of detection, limit of quantification, accuracy, and precision of the proposed methods were also evaluated.

• Journal of The Korean Society of Grassland and Forage Science
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• v.36 no.4
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• pp.333-339
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• 2016

The objective of this study was to optimize analytical methods for ochratoxin A (OTA) and zearalenone (ZEA) in rice straw silage and winter forage crops using ultra-high performance liquid chromatography (UHPLC). Samples free of mycotoxins were spiked with $50{\mu}g/kg$, $250{\mu}g/kg$, or $500{\mu}g/kg$ of OTA and $300{\mu}g/kg$, $1500{\mu}g/kg$, or $3000{\mu}g/kg$ of ZEA. OTA and ZEA were extracted by acetonitrile and cleaned-up using an immunoaffinity column. They were then subjected to analysis with UHPLC equipped with a fluorescence detector. The correlation coefficients of calibration curves showed high linearity ($R^2{\geq_-}0.9999$ for OTA and $R^2{\geq_-}0.9995$ for ZEA). The limit of detection and quantification were $0.1{\mu}g/kg$ and $0.3{\mu}g/kg$, respectively, for OTA and $5{\mu}g/kg$ and $16.7{\mu}g/kg$, respectively, for ZEA. The recovery and relative standard deviation (RSD) of OTA were as follows: rice straw = 84.23~95.33%, 2.59~4.77%; Italian ryegrass = 79.02~95%, 0.86~5.83%; barley = 74.93~97%, 0.85~9.19%; rye = 77.99~96.67%, 0.33~6.26%. The recovery and RSD of ZEA were: rice straw = 109.6~114.22%, 0.67~7.15%; Italian ryegrass = 98.01~109.44%, 1.65~4.81%; barley = 98~113.53%, 0.25~5.85%; rye = 90.44~108.56%, 2.5~4.66%. They both satisfied the standards of European Commission criteria (EC 401-2006) for quantitative analysis. These results showed that the optimized methods could be used for mycotoxin analysis of forages.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.327-334
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• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.16-24
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• 2011

A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

• Journal of Sericultural and Entomological Science
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• v.47 no.2
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• pp.51-55
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• 2005

Resveratrol is naturally occurring phytoalexin compounds produced by grape berries, peanuts, and their products in response to stress such as fungal infection, heavy metal ions or UV irradiation. The objective of this study was to develope a reliable high performance liquid chromatographic (HPLC) method for the quantitative determination of trans-resveratrol in mulberry fruit. Samples were extracted in 80% MeOH and filtered with $0.45{\mu}m$ syringe filter. The transresveratrol was separated Waters $C_{18}$ column, using a mobile phase containing 0.025% trifluroacetic acid in 5% acetonitril and 0.035% trifluroacetic acid in 50% acetonitril, detected by photodiode array detector (PDA) at 254 nm and the flow rate was 1ml/min. Under this analytical condition, the mean content of mulberry fruits (fifty varieties) was $777.3{\pm}585.9ppm$. Among the tested samples, 'Mansaengbaekpinosang (II)' was the highest level in 3450.6 ppm. However four accessions including 'Gukbu', 'Sabangso (I)', 'Simseol' and yield mulberry fruit were not able to detected. Eight suitable varieties selected for the production of fruit were 'Jeolgokchosaeng (Chungbuk)' 777.8 ppm, 'Dangsang 7' 771.1 ppm, 'Jangsosang' 133.9 ppm, 'Susungppong' 31.1 ppm, 'Suwonnosang' 639.7 ppm, 'Palcheongsipyung' 1475.9 ppm, 'Kangsun' 864.0 ppm, and 'Jukcheonchosaeng' 1458.5 ppm. 'Daesungppong' which was the first authorized variety for the production of mulberry fruit was 1236.7 ppm. In conclusion, these results suggest that mulberry including fruit and leaf may a good new resource for resveratrol production.

• Korean Journal of Food Science and Technology
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• v.45 no.6
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• pp.693-699
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• 2013

A simple, sensitive, and specific method for quantifying the nicotine content of synthetic favoring substances (SFS) was developed using high performance liquid chromatography (HPLC) with a photo-diode array detector (PDA). Nicotine was extracted from SFS samples by using an acid-base liquid-liquid extraction method with dichloromethane and distilled water. The nicotine content was quantified by HPLC/PDA (261.9 nm) with a $C_{18}$ column under a gradient of 10% acetonitrile with 20 mM ammonium formate (ammonia solution adjusted to pH 8.7) to 100% acetonitrile. The calibration curve, analyzed from concentration standards between 0.1 to 2 mg/L, presented linearity with a correlation coefficient ($r^2$)>0.9999. The limit of quantitation (LOQ) of nicotine in SFS was 0.4 mg/kg, and the average recoveries ranged from 76.4% to 96.3%. The repeatability of measurements, expressed as the coefficient of variation (CV%), ranged from 1.74 to 5.12%. This newly developed method for nicotine quantification in SFS can be considered an analytical method with an acceptable level of sensitivity and repeatability.