• Korean Journal of Environmental Agriculture
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• v.38 no.4
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• pp.321-331
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• 2019

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C₁₈. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Korean Journal of Environmental Agriculture
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• v.42 no.1
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• pp.71-81
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• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Korean Journal of Food Science and Technology
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• v.40 no.6
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• pp.603-610
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• 2008

The principal objective of current study was to evaluate the potential of near infrared reflectance spectroscopy (NIRS) as a non-destructive method for the prediction of the amylose and protein contents of un-hulled and brown rice in broad-based calibration models. The average amylose and protein content of 75 rice accessions were 20.3% and 7.1%, respectively. Additionally, the range of amylose and protein content were 16.6-24.5% and 3.8-9.3%, respectively. In total, 79 rice germplasms representing a wide range of chemical characteristics, variable physical properties, and origins were scanned via NIRS for calibration and validation equations. The un-hulled and brown rice samples evidenced distinctly different patterns in a wavelength range from 1,440 nm to 2,400 nm in the original NIR spectra. The optimal performance calibration model could be obtained by MPLS (modified partial least squares) using the first derivative method (1:4:4:1) for un-hulled rice and the second derivative method (2:4:4:1) for brown rice. The correlation coefficients $(r^2)$ and standard error of calibration (SEC) of protein and amylose contents for the un-hulled rice were 0.86, 2.48, and 0.84, 1.13, respectively. The $r^2$ and SEC of protein and amylose content for brown rice were 0.95, 1.09 and 0.94, 0.42, respectively. The results of this study suggest that the NIRS technique could be utilized as a routine procedure for the quantification of protein and amylose contents in large accessions of un-hulled rice germplasms.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2001.06a
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• pp.1622-1622
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• 2001

The purpose of this research was to develop a the reflection technique with near infrared (NIR) radiation for estimating physico-chemical properties in compost. The composts (cattle, pig, chicken and waste composts) were air dried and then ground to pass through a 0.5 or 2mm sieve for the physico-chemical properties and spectroscopic determinations. The physico-chemical properties of compost were shown high values ; moisture(30-60%), T-N(0.8-2.9%), organic matter(29-89%), pH(5.89-9.60) K$_2$O(0.27-5.66%), P2O$\sub$5/(0.07-2.62%), CaO(0.03-4.80%), MgO(0.09-1.56%), NaCl(0.01-1.13%), EC(1.41-13.76dS/m). Generally, we should select a simple calibration and prediction method for determining physico-chemical properties in compost under similar accuracy and precision of prediction. It should be remembered that the NIRS approach will never replace the traditional methods. However, NIRS technique may be an effective method for rapid and nondestructive measurements of a large number of compost samples. Near infrared reflectance spectra of composts was obtained by Infra Alyzer 500 scanning spectrophotometer at 2-nm intervals from 1100 to 2500nm. Multiple linear regression(MLR) or partial least square regression (PLSR) was used to evaluate a NIRS method for the rapid and nondestructive determination of physico-chemical properties and humic acid contents in composts. The standard error of prediction(SEP) for finely sized sample(<0.5mm) and coarsely sized sample(<2mm) did not show much difference. The NIR instrument of filter type showed the same accuracy of the monochromator scanning type to estimate the compost properties. The results summarized that NIR spectroscopy can be used as a routine testing method to determine quantitatively the OM, moisture, T-N, color, pH, cation content in the compost samples nondestructively.

• Korean Journal of Soil Science and Fertilizer
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• v.34 no.4
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• pp.278-283
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• 2001

The overall objective of this research was to show a NIR soil analyzer assessing soil fertility by measuring soil properties rapidly. A total of 140 soil samples were used to obtain calibrations and validation estimating soil properties. The soil samples were ground to pass 0.2mm sieve openings. Partial least square regression analysis was used to develop a calibration for soil analysis. The results indicated that NIR soil analyzer could be used as a routine method for quantitatively determining pH, OM, total nitrogen, CEC, extractable Ca, Mg, K, available $SiO_2$ and soil moisture simultaneously within one minute. Therefore, the NIR soil analyzer may be suitable for quick estimation of soil fertility estimation in fertilizer assessments.

• Korean Journal of Soil Science and Fertilizer
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• v.34 no.4
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• pp.273-277
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• 2001

Traditional methods of chemical analysis for the soil properties take time and produce harmful waste. The purpose of this research was to evaluate an NIR technique for measuring some soil properties that are rapid and accurate in soil fertility assessments. The NIR instrument (InfraAlyzer 500, Bran & Luebbe Co.) was used for obtaining spectral data from 140 finely ground soil for calibrations and validation estimating pH, CEC, extractable Ca, Mg, K, $SiO_2$, humic acid and EC. Partial least square regression analysis was used to develop a calibration of NIR spectroscopy method. The results indicated that NIR spectroscopy could be used as a routine nondestructive method quantitatively determining soil chemical properties quickly. However the NIR technique may require sample preparation to obtain even diffuse reflection spectra from the soil and data manipulations to obtain optimal predictions.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.29 no.2
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• pp.76-82
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• 1997

In paper the evenness of planar distribution of mass in a small scale is called formation (orbetter:mass formation). Traditionally formation has been assessed visually, by looking the sheet of paper against transmitted light. Different kinds of optieal testers are being usd to obtain quantitative rankings htat would be independent of the observer but would well correspond to the visual assessment. However, various raw-material and process factors do influence light trans-mittance in paper and do impair the correspondence between basis weight and the optical formation measurement (or visual assessment). As the optical formation test methods do not incorporate an efficient calib ration routine, the formation of the sophisticated paper grades of today the is rather difficult to measure optically and may lead to erroneous results. It may be concluded that the optical measurement is not suitable for paper grades with high filler content. coating, heavy calendering or that are made of heavily beaten pulp, nordoes it apply for dyed or printed papers. For this reason, visual assessment and optical evaluation shoild be replaced with a measurement that gives reliable results independent on paper grode and manufacturing process. Formation measuremend based on beta radiation is suitable for all paper grades regardless to the material contents or process treatment. It is possible to measure even dyed or printed samples. Thonks to a sim ple and relioble calibration, the results are converted to real basis weight balues that remain reliable even with time. The only beta tester commercially available is the AMBERTEC Beta Formation Tester. Formation of paper does vary locally in the web. Typically there exists a formation profile, too similarly to other properties of paper. Therefore, formation should ？ ays be expressed as a mean of a sufficient amount of parallel determinations. All formation measurements should be calibrated against basis weight.

• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3629-3634
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• 2013

In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

• Journal of The Korean Society of Inherited Metabolic disease
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• v.15 no.3
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• pp.138-146
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• 2015

Purpose: If early diagnosis is not made, patients with metabolic disorders as homocystinemia rapidly progress to physical defect or mental retardation resulted in storage of the toxic material into the brain. Therefore, it is necessary to develop an analytical method for a rapid screening and/or correct confirmation diagnosis. Methods: The standard solution of sulfur amino acids spiked plasma was subjected to protein precipitation with methanol, and then consecutively derivatized with trimethylsilyl (TMS) and trifluoroacyl (TFA) and determined by GC-MS. The formation of TMS derivative of the hydroxyl and TFA derivative of amino functional group was performed by BSTFA and MBTFA, respectively. Selective ion monitoring (SIM) mode was used for quantification with selected specific ions. Results: A calibration curve on standard spiked pooled plasma showed a linear relationship with correlation coefficient of 0.9936-0.9992 for all compounds over the range of 0.1-300 ng. The precision and accuracy were within S.D. of 1-15% and RSD of 1-15% for intra-day assay at 2 ng/mL, 15 ng/mL and 30 ng/mL. LOD and LOQ was 0.4 ng/mL and 4 ng/mL respectively. Conclusion: A rapid analytical method was developed to quantify sulfur amino acids and methyl malonic acid, after two-step derivatization procedure with good sensitivity and specificity on human plasma. Advantages of a new method are simplicity and rapidity. The method could be useful for routine analysis, diagnosis of homocysteinemia.

• Bulletin of the Korean Chemical Society
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• v.25 no.3
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• pp.365-372
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• 2004

Two simple, rapid and sensitive spectrophotometric methods for the determination of three fluoroquinolones, namely levofloxacin, norfloxacin and ciprofloxacin have been performed either in pure form or in their tablets. In the first method, levofloxacin and norfloxacin are directly treated with bromocresol green (BCG) in dichloromethane while ciprofloxacin is allowed to react with the same dye in aqueous acidic buffer. Highly yellow colored complex species were formed instantaneously in case of levofloxacin and norfloxacin or after extraction into dichloromethane for ciprofloxacin. The formed complexes are quantified spectrophotometrically at their absorption maxima at 411 nm for levofloxacin and 412 nm for norfloxacin and ciprofloxacin. The second method involves the reaction of levofloxacin with ${\rho}$-chloranilic acid ( ${\rho}$-CA) and norfloxacin with tetracyanoethylene (TCNE) in acetonitrile to give complexes with maximum absorbance at 521 and 333 nm for the two drugs, respectively. Adopting the first procedure, calibration graphs were linear over the range 1- 20 ${\mu}g\;mL^{-1}$ with mean percentage recoveries of 100.41 ${\pm}$ 0.72, 99.99 ${\pm}$ 0.54 and 100.23 ${\pm}$ 0.91 for the theree drugs, respectively. For the second procedure, the concentration ranges were 15-250 ${\mu}g\;mL^{-1}$ for levofloxacin using ${\rho}$-CA and 0.8-16 ${\mu}g\;mL^{-1}$ for norfloxacin using TCNE with mean percentage recoveries of 99.88 ${\pm}$ 0.45 and 100.26 ${\pm}$ 0.68 for the two drugs, respectively. The proposed methods were successfully applied to determine these drugs in their tablet formulations and the results compared favorably to that of reference methods. The proposed methods are recommended for quality control and routine analysis.