• Weed & Turfgrass Science
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• v.1 no.4
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• pp.44-49
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• 2012

The objective of this study was to know the herbicidal activity of the essential oil from amyris (Amyris balsamifera). In a seed bioassay experiment, the amyris essential oil inhibited the growth of rapeseed (Brassica napus) by fifty percent at 8.8 ${\mu}g\;g^{-1}$. And in a greenhouse experiment, sorghum, barnyard grass and Indian jointvetch, which was applied in above-ground parts, with the amyris essential oil at 4,000 ${\mu}g\;ml^{-1}$ showed visual injuries of 90, 70, and 70, respectively (0, no damage; 100, total damage). However, soil application of the essential oil did not show such herbicidal injuries. In a field experiment, foliar application of the amyris essential oil at 5% controlled effectively weeds such as barnyardgrass, shepherd's purse, and clover in 24 hours. Our results indicated that the amyris essential oil had herbicidal activity. To understand the composition of the amyris essential oil, the oil was analyzed by gas chromatography-mass spectometry with solid-phase micro-extraction apparatus. There were 15 organic chemicals in the oil and the major constituents were calarene, elemol, ${\gamma}$-eudesmol, curcumene, ${\beta}$-sesquiphellandrene, zingiberene, selina-3,7(11)-diene, 1,3-diisopropenyl-6-methyl-cyclohexene, ${\beta}$-bisabolene, and ${\beta}$-maaliene. Overall results suggest that the amyris essential oil had a herbicidal activity with fast, contact, and non-selective mechanism.

• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.110-117
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• 2018

The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.118-123
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• 2018

The objective of this study was to develop a sensitive method for the identification and determination of nitrovin in fishery products by using a solid-phase extraction (SPE), as performed with a liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with a mixture of acetonitrile and water, and were then defatted with acetonitrile saturated hexane, after which further clean-up was accomplished with SPE on the hydrophilic-lipophilic balance (HLB) cartridges. The analytes were subsequently ionized in the positive mode of an electrospray ionization (ESI), and where thereby detected in a process of multiple reaction monitoring (MRM). The linearity (expressed as correlation coefficients) of the matrix calibration curves was > 0.985. The limit of the quantification for the nitrovin was measured at 0.001 mg/kg. The accuracy (expressed as average recovery) was noted between 72.1 and 122%. The precision (expressed as coefficient variation) was noted from 2.9 to 16.9%. According to the CODEX CAC/GL-71 guideline accuracy, precision, linearity, and limit of detection were determined in three matrices (which were flatfish, eel and shrimp). The proposed method was suitable for analyzing the associated nitrovin residues. This application and result can also be a factor to contribute to the non-detection drugs management in fishery products.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.141-146
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• 2017

A rapid and precise method using LC-MS/MS was developed for carbendazim analysis in agricultural products. This compound was extracted with acetonitrile from agricultural products and cleaned up by solid-phase extraction procedure. The limit of detection and quantification were 0.001 mg/kg and 0.004 mg/kg, respectively. The mean recoveries and precision from 4 agricultural products, soybean sprout and mungbean sprout were in the range of 83.3-86.4% and 0.2-3.0% spiked at 1.0 mg/kg and those were in the range of 77.3-90.1% and 1.3-3.8% spiked at 0.02 mg/kg. The present method is faster and more precise compared with the multi-residue method of Korean Food Code. Therefore, we conclude that this method is suitable for carbendazim determination in a wide range of agricultural products.

• Journal of Life Science
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• v.29 no.2
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• pp.198-201
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• 2019

Recently, it has been reported that Bacillus mojavensis possesses antifungal properties and plant growth-promoting activities, which are similar to the characteristics of siderophore. In this study, the siderophore produced by B. mojavensis was assessed using a solid phase extraction (SPE) cartridge and liquid chromatography quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). After B. mojavensis was incubated in phenol medium for 16 hr and lyophilized, the sample was dissolved in water and loaded to an SPE cartridge to remove interferences. The cartridge was washed with 5% methanol in water and eluted with 2% formic acid in methanol sequentially. The eluted solution was evaporated under a stream of nitrogen gas and reconstituted in methanol. The reconstituted sample was filtered, and $1{\mu}l$ of the sample was assessed using Q-TOF MS/MS. The mass spectrometer was operated using the positive electrospray ionization mode. Based on the mass spectrum and tandem mass spectrum, the siderophore produced by B. mojavensis was bacillibactin, one of the catechol types of siderophore with a molecular weight of 882.2556. This siderophore analysis could provide a justification for the study of B. mojavensis as a functional food and for pharmaceutical applications.

• Journal of Applied Biological Chemistry
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• v.64 no.2
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• pp.177-184
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• 2021

While veterinary antibiotics are used only in a part of the dose administered, the rest are excreted as urine or feces. Residual antibiotics enter the adjacent agricultural environments by spraying manure-based composts on farmlands and lead to secondary pollution. Therefore, it is necessary to develop the technique for post management such as regulatory levels of antibiotics in the agricultural environments. This study was conducted to compare by different matrices the amount of residual antibiotics such as tetracyclines and sulfonamides, which are known to be frequently used in Korea and to practice risk assessment by different antibiotics in soils before and after application of composts. Pre-treatment with modified typical method using buffer and solid phase extraction showed the recovery of composts and soils was more than 70% at ppb level and the limits of detection were 0.13-0.46 and 0.05-0.25 ㎍/kg, respectively. Analysis of manure-based composts revealed concentrations from 5.38 to 196.0 ㎍/kg for tetracyclines, from below the detection of limit (BDL) to 259.0 ㎍/kg for sulfonamides. In case of agricultural soils, residual concentrations of selected veterinary antibiotics were ranged 0.30-53.3 ㎍/kg, BDL-4.16 ㎍/kg respectively and the concentration level of tetracyclines, which had higher soil distribution coefficient (Kd) values, was higher than that of sulfonamides. There was a difference in human risk assessment by different antibiotics in soil before and after application of composts. But, it was indicated that detection values of all of 5 antibiotics were very safe on the basis that Hazard Quotient was safe below 1.

• Journal of Applied Biological Chemistry
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• v.65 no.1
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• pp.17-21
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• 2022

A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH₂) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r²) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

• Analytical Science and Technology
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• v.21 no.6
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• pp.535-542
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• 2008

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

• Journal of the Korean Society of Food Culture
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• v.22 no.2
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• pp.246-253
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• 2007

Mineral and volatile flavor compounds of Pimpinella brochycarpa N., a perennial Korean medicinal plant of the Umbelliferae family, were analyzed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and simultaneous steam distillation extract (SDE)-gas chromatography mass spectrometry (GC/MS), head space solid phase micro-extraction (HS-SPME)-GC/MS. Mineral contents of the stalks and leaves were compared and the flavor patterns of the fresh and the shady air-dried samples were obtained by the electronic nose (EN) with 6 metal oxide sensors. Principal component analysis (PCA) was carried out using the data obtained from EN. The 1st principal values of the fresh samples have + values and the shady air-dried have - values. The essential oil extracted from the fresh and the shady air-dried by SDE method contain 58 and 31 flavor compounds. When HS-SPME method with CAR/PDMS fiber and PDMS fiber were used, 34 and 21 flavor compounds. The principal volatile components of Pimpinella brachycarpa N. were ${\alpha}$-selinene, germacrene D, and myrcene.

• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.