• Toxicological Research
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• v.31 no.3
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• pp.255-264
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• 2015

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.

• Journal of Korean Society of Environmental Engineers
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• v.38 no.10
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• pp.535-542
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• 2016

As one of the most cost-effective methods for surface emission measurements, flux chamber method has been used worldwide. It can be classified into two types: SFC (with slope method) and DFC (with steady-state method). SFC (static flux chamber) type needs only simple equipment and is easy to handle. However, the value of flux might vary with SFC method, because it assumes that the change of concentration in chamber is linear with time. Although more specific equipments are required for DFC (dynamic flux chamber) method, it can lead to a constant result without any ambiguity. We made a self-designed DFC using a small and compact kit, which recorded good sample homogeneity (RSD < 5%) and recovery ( > 90%). Relative expanded measurement uncertainty of this improved DFC method was 7.37%, which mainly came from uncontrolled sweep air. The study shows that the improved DFC method can be used to collect highly reliable emission data from large landfill area.

• Journal of Pharmaceutical Investigation
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• v.39 no.1
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• pp.29-36
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• 2009

Since the quality of final products is significantly affected by the homogeneity of powder mixture, the powder blending process has been regarded as one of the critical pharmaceutical unit processes, especially for solid dosage forms. Accordingly, the monitoring to determine a blending process' end-point based on a faster and more accurate in-line/on-line analysis has attracted enormous attentions recently. Among various analytical tools, NIR (near-infrared) spectroscopy has been extensively studied for PAT (process analytical technology) system due to its many advantages. In this study, NIR spectroscopy was employed with an optical fiber probe for the in-line monitoring of fluid-bed blending process. The position of the probe, the ratio of binary powder mixture, the powder size differential and the back-flush period of the shaking bag were examined as principal process parameters. During the blending process of lactose and mannitol powders, NIR spectra were collected, corrected, calibrated and analyzed using MSC and PLS method, respectively. The probe position was optimized. A reasonable end-point was predicted as 1,500 seconds based on 5% RSD value. As a consequence, it was demonstrated that the blending process using a fluid-bed processor has several advantages over other methods, and the application of NIRS with an optical fiber probe as PAT system for a fluid-bed blending process could be high feasible.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.361-369
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• 2015

This study investigated residual characteristics of bistrifluron and fluopicolide in Korean cabbage, and suggested the pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The pesticides were sprayed on Korean cabbage in two different region under greenhouse conditions at the recommended dose, respectively. The samples for residue analysis were harvested at 0 (2 hr), 1, 2, 4, 6, 8 and 10 days after treatment, and analyzed by HPLC after clean-up with Florisil SPE. The limit of quantification (LOQ) was $0.03mg\;kg^{-1}$ for bistrifluron and fluopicolide, and the recoveries ranged from 87.2-110.6% with below 5% of RSD. The biological half-lives of field I and field II were 3.9 and 4.2 days for bistrifluron and 4.9 and 4.2 days for fluopicolide, respectively. The PHRL of bistrifluron and fluopicolide were recommended as 3.83 and $3.23mg\;kg^{-1}$ for 10 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.296-313
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• 2014

A QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) multiresidue method was developed for the simultaneous analysis of 124 pesticides in soil by LC-MS. The procedure involved liquid extraction of soil immersed with 0.2N $NH_4Cl$ by acetonitrile with 1% acetic acid, followed by anhydrous $MgSO_4$ and sodium acetate, and dispersive SPE cleanup with $MgSO_4$, primary secondary amine (PSA) and $C_{18}$. The extracts were analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.99. Recovery studies for the validation were carried out using two type soils, loam and sandy loam, at four concentration levels (0.005, 0.01, 0.02, and 0.1 mg/kg). The recoveries of pesticides were in the range of 70-120% with < 20% RSD except 4 pesticides, Benfuracarb, Ethiofencarb, Pymetrozine, and Pyrethrin. This result indicated that the method using QuEChERS and LC-MS/MS could be applied for the simultaneous determination of pesticide residues in soils.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.278-295
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• 2014

Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

• Analytical Science and Technology
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• v.23 no.1
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• pp.24-35
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• 2010

To learn more about the calibration properties of reduced sulfur compounds (RSCs) by the combination of gas chromatography(GC)-pulsed flame photometric detector (PFPD) and thermal desorption method, a series of calibration experiments were conducted on the basis of both internal and external calibration approaches. For these experiments, gaseous standards of 4 RSCs ($H_2S$, $CH_3SH$, DMS, and DMDS) were prepared at two different concentration levels of both low (10, 20, 50,and 100 ppb) and high ranges (100, 200, 500, and 1000 ppb) along with $CS_2$ as an internal standard. First, the external calibration results were compared between fixed standard volume (FSV) and fixed standard concentration (FSC) method. Secondly, FSV-based calibration results were compared between external and internal calibration results. As FSV method suffers from sensitivity variations less significantly than FSC, the former is recommended to maintain the consistency in GC-TD sensitivity for RSC analysis. In addition, when the calibration data were examined in terms of RSE between external and internal calibration data, the results were not consistent enough to show improvements in internal method. Hence, diverse efforts are desirable to optimize the reproducibility in terms of GC-TD sensitivity for RSC analysis.

• Analytical Science and Technology
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• v.27 no.4
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• pp.201-212
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• 2014

Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted in consumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extraction and quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumer products as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of a bag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of the standard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standard curves for all 18 PAHs were obtained with $R^2$ above 0.999. Precisions of the retention times and the peak areas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. The recoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solvents such as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymer samples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and 1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three samples while 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations of maximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are needed to decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstrate cases that the clean up is required.

• Analytical Science and Technology
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• v.26 no.2
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• pp.142-153
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• 2013

A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl ($NH_2$) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient ($R^2$) of both lepimectin $A_3$ and $A_4$ solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate, rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

• Analytical Science and Technology
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• v.31 no.2
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• pp.78-87
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• 2018

Asian lacquer has been used as an adhesive and coating material in Asian countries, such as China, Japan, and Korea, and other southeast Asian countries. In this study, the changes in the chemical structure of lacquer with drying was analyzed using pyrolysis/GC/MS (which is useful in analyzing polymeric material) to understand its drying procedures. Upon increasing temperature, the dried lacquer was fully pyrolyzed above the pyrolysis temperature of $500^{\circ}C$. The repeatability was good at the pyrolysis temperature of $500^{\circ}C$ (rsd = 2.6-22.3 %); however, there were differences in the pyrogram patterns when the difference in sample quantity was large. The characteristic peaks of Asian lacquer components, such as those corresponding to 1,2-benzenediol and 3-methyl-1,2-benzenediol, were detected and the compound of each peak was assigned according to the mass library. As the lacquer dried, the composition of pyrolysis products with urushiol derivatives bearing 3 C=C bonds was severely reduced compared with the ones with no C=C bonds, indicating that the polymerization is related to C=C bonds. These results can be applied to confirm the presence of lacquer in excavated relics and to monitor the changes in the composition of raw lacquer with drying.