• KSBB Journal
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• v.31 no.1
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• pp.1-7
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• 2016

Changes in the concentrations of glucosinolates and related compounds in different extracts of Dolsan leaf mustard kimchi (DLMK) and Dolsan leaf mustard pickles (DLMP) were during storage investigated. Samples were kept at 0oC for 35 days and collected at 7 day intervals. The leaves and stems of DLMK and DLMP were refluxed for 24 h with 50% acetonitrile, and the extracts were analyzed by LC-PDA/MS/MS. The main glucosinolates detected in DLMK were sinigrin, gluconapoleiferin, glucobrassicanapin, and gluconapin, whereas those in DLMP were sinigrin, gluconapoleiferin, glucobrassicanapin, glucobrassicin, and glucoerucin. Sinigrin concentrations were quantified by UV absorption at 228 nm. Sinigrin concentrations in the leaves and stems of DLMK on the day of preparation were 2.14 mg/g and 2.25 mg/g, respectively, and those on day 35 after preparation were 1.25 mg/g and 1.00 mg/g, respectively. DLMP showed a similar trend: the concentrations in the leaves and stems on the day of preparation were 2.04 mg/g and 0.29 mg/g, respectively, whereas those on day 35 after preparation were 0.59 mg/g and 0.41 mg/g, respectively. Thus, sinigrin concentrations decreased during storage.

• KSBB Journal
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• v.31 no.1
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• pp.20-26
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• 2016

This study aims to examine the optimum blanching conditions as a pretreatment condition to improve the storage stability of Dolsan leaf mustard pickle. The effects of the blan- ching temperature and time were investigated at a temperature range of $80-100^{\circ}C$. Sampling was done for 1 month after a 5 days interval. The L value of the Dolsan leaf mustard was found to be the highest at $80^{\circ}C$. The cutting force increased as the blanching temperature increased. The tensile strength decreased at $95^{\circ}C$ and $100^{\circ}C$. In addition, the sensory evaluation scores were the best at $80^{\circ}C$. The storage stability was assessed at various blanching temperatures to increase the sinigrin content during storage. Liquid chromatography with photodiode array and tandem mass spectrometry (LC-PDA/MS/MS) analysis was conducted to identify and quantify the sinigrin content in the Dolsan leaf mustard. Sinigrin as an internal standard was co-injected into each sample solution. The sample was monitored by recording the ultraviolet absorbance at 228 nm and by electrospray ionization (ESI) positive ion mode in the m/z 50-1,500 range. Blanching the sample at $80^{\circ}C$ showed the highest sinigrin concentration during storage among various temperatures and the maximum concentration was 350 ppm at 15 days storage. Study on utilization of vegetable from food processing of leaf mustard and preservation conservation results suggest that blanching at $80^{\circ}C$ is expected to improve the palatability of the pickle.

• Natural Product Sciences
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• v.24 no.3
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• pp.206-212
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• 2018

Xanthii Fructus has been traditionally used for the treatment of rhinitis, rheumatoid arthritis, and eczema. In this study, a high-performance liquid chromatography-photodiode array (HPLC-PDA) method was developed and then used for the simultaneous analysis of eight phenylpropanoids in Xanthii Fructus. The analytical column used for this separation was a $SunFire^{TM}$ $C_{18}$ column, maintained at $40^{\circ}C$. The mobile phase used was 1.0% acetic acid in distilled water and 1.0% acetic acid in acetonitrile with gradient elution. For identify of each component, the mass spectrometer (MS) was used a Waters triple quadrupole mass spectrometer requipped with electrospray ionization (ESI) source. The HPLC-PDA method showed good linearity: correlation coefficients were ${\geq}0.9996$. The limits of detection and quantification of the eight compounds were 0.02 - 0.04 and $0.06-0.14{\mu}g/mL$, respectively. The extraction recoveries ranged from 97.51 to 108.67%. The relative standard deviation values of intra- and inter-day precision were 0.06 - 1.55 and 0.09 - 1.68%, respectively. The validated HPLC-PDA method was applied to simultaneously analyse the amounts of eight phenlypropanoids in Xanthii Fructus.

• Analytical Science and Technology
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• v.34 no.4
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• pp.172-179
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• 2021

Oleanane-type triterpenoids exist as secondary metabolites in various plants. In particular, soyasaponin, an oleanane-type triterpenoid, is abundant in the hypocotyl of soybean, one of the most widely cultivated crops in the world. Depending on their chemical structure, soyasaponins are categorized as group A saponins or group DDMP (2,3-dihydro-2,5-dihydroxy-6-methyl-4H-pyran-4-one) saponins. The different soyasaponin chemical structures present different health functionalities and taste characteristics. However, conventional phenotype screening of soybean requires a substantial amount of time for functionality of soyasaponins. Therefore, we attempted to use liquid chromatography with a photodiode array detector and tandem mass spectrometry (LC-PDA/MS/MS) for accurately predicting the phenotype and chemical structure of soyasaponins in the hypocotyl of five common soybean natural mutants. In this method, the aglycones (soyasapogenol A [SS-A] and soyasapogenol B [SS-B]) were detected after acid hydrolysis. These results indicated that the base peak and fragmentation differ depending on the chemical structure of soyasaponin with aglycone. Thus, a fragmentation database can help predict the chemical structure of soyasaponins in soyfoods and plants.

• Korean Journal of Food Science and Technology
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• v.43 no.6
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• pp.675-682
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• 2011

This study was conducted to monitor the concentrations of 24 anti-impotence drugs and their analogues in various foods and dietary supplements, with the aim of ensuring the safety of the foods and supplements. The measurements were done in 226 samples using high performance liquid chromatography/photodiode array detector (HPLC/PDA) and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Five male sexual function enhancing products have been detected as follows: acethylvardenafil (21,476 mg/kg; 15 mg/capsule from one sample), sildenafil (52,778 mg/kg, 29 mg/capsule in one sample; 71,535 mg/kg, 48 mg/capsule in one sample), and tadalafil (9,772-55,545 mg/kg, 6-33 mg/capsule in four samples). A sustainable monitoring of anti-impotence drugs and their analogues in various foods and dietary supplement is recommended.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.242-256
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• 2012

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

• 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.

• Journal of Food Hygiene and Safety
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• v.18 no.4
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• pp.195-201
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• 2003

An easily available, simultaneous identification/determination procedure for sildenafil, homosildenafil, tadalafil, vardenafil in adulterated health related foods was established by using a combination of three different analytical methods; thin layer chromatography(TLC), liquied chromatography-mass spectrometry (LC/MS) and high-performance liquied chromatography (HPLC)/photo-diode-array detector. The sample solution for TLC was applied to silica gel 60 $F_{254}$ plates with ethylacetate/acetonitrile/25%ammonia (90:10:5) as a developing solvent. Spots were located under UV radiation at 254 nm and dragendolfs reagent. Mass spectra of the compounds by LC/MS were investigated with electrospray ionization (ESI) interface, under positive ion mode. The HPLC analysis was performed on a column of capcell pack $C_{18}$ (UG120, 4.6${\times}$250mm I.D. 5 ${\mu}$m)with 0.1% sodium 1-hexansulfonate (in 0.1% phosphoric acid)/acetnitrile (73:27) as a mobile phase, and effluent was minitored with a photo-diode-applied to commercial foods, Sildenafil content was inthe range of 0.4mg/g~360.9 mg/g from 7 out of 35 samples. Homosildenafil content was in the range of 2.2 mg/g~336.0 mg/g from 7 out of 35 samples. Tadalafil content was 429.3 mg/g, 9.6 mg/500 mg from 2 out of 35 samples. The procedure described here is available for the screening of sildenafil, homosildenafil, tadalafil, vardenafil.

• Korean Journal of Food Science and Technology
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• v.48 no.5
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• pp.405-412
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• 2016

Illegally adulterated compounds, such as impotency drugs and their synthetic analogues, which have been purported to enhance sexual potency or mood, have been constantly detected in foods including dietary supplements. The adulterated foods with these illegal compounds may threaten public health because their safety and efficacy have not been verified. This study was aimed at investigating illegal compounds in foods and counterfeit products. 54 illegal compounds were assayed using a simultaneous analytical method involving liquid chromatography equipped with photo diode array (LC-PDA) and LC coupled with tandem mass spectrometry (LC-MS/MS). The method was validated in terms of selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision and accuracy. In 48 of 161 samples, we identified 7 different illegal compounds, including sildenafil, tadalafil, chlropretadalafil, demethylsildenafil, dimethyl-thiosildenafil, icariin and yohimbine. When purchasing products marketed for erectile dysfunction or aphrodisiacs, ulmost care should be taken owing to the possible presence of these illegal compounds.

• Analytical Science and Technology
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• v.22 no.4
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• pp.345-353
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• 2009

The new anti-impotency analogue was identified in food source. Detection of this analogue was accomplished through screening of food samples by liquid chromatography/photodiode array detector. The spectrum pattern of analogue compound was similar to that observed for hongdenafil which was analogue of sildenafil. This new compound was isolated and purified using the liquid-liquid extraction, thin layer chromatography, column chromatography and preparative HPLC. And then those structure were identified using analytical instruments such as HPLC/PDA, LC/MS/MS and NMR. The compound was given a name to oxohongdenafil which was replaced with acetyl oxoethylpiperazinyl residue instead of sulfonyl piperazine group of sildenafil. The regulation for the abovementioned analogue, oxohongdenafil, was established by Standard of Korean food code.