• Bulletin of the Korean Chemical Society
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• v.29 no.6
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• pp.1185-1189
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• 2008

Two HPLC methods such as cefadroxil and cefalexin methods were compared in their performance for the quantitative analysis of the content and purity of $\beta$ -lactamic antibiotic, cefradine, for six bulk drug samples. Between the two methods, the cefadroxil method prescribed by the European Pharmacopoeia (EP) for the determination of impurities in cefradoxil was superior to the cefalexin method prescribed by the EP and by the United States Pharmacopeia (USP) for the determination of cefalexin impurity in cefradine in terms of the greater stability of the chromatogram baselines and the higher precision, i.e., the lower % relative standard deviation (RSD). Based on the comparison of the two HPLC methods, the cefadroxil method was recommended to replace the TLC method, which has been prescribed by the EP as the official method for determination of extraneous impurities in cefradine.

• Microbiology and Biotechnology Letters
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• v.18 no.1
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• pp.18-25
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• 1990

Paralytic Shellfish Poison (PSP) is mainly produced by marine dinoflagellates such as Protogonyaulax sp. and Pyrodinium sp.. The PSP was known to be accumulated in digestive gland of shellfish as result of feeding toxic dinoflagellates. PSP illness when occurs when one eats PSP intoxicated shellfish. Therefore PSP is becoming as serious problem in food hygiene and shellfish cultivation industry. The purpose of this study was to develop detoxification method for utilization of PSP intoxicated sea mussel and prevent from PSP illness. The PSP was extracted with 0.1 N HCl solution from the submitted sea mussel, then the toxicity was measured by mouse assay according to Official Methods of Analysis of the Association of Official Analytical Chemists. No detoxification effect was observed by adding extracted juice of garlic and ginger. When the sea mussel homogenate was heated at various temperatures, the PSP toxicity was not changed significantly at below $70^{\circ}C$ for 60 minutes but it was decreased as the heating temperature was increased. For example, when the sea mussel homogenate was heated at 100, $121^{\circ}C$ for 10 minutes, the toxicity was decreased about 67 and 90%, respectively. When the sea mussel containing 645 $\mu$g PSP per 100g of edible meat was processed according to general shellfish canning procedure, the toxicity was decreased as the level of PSP undetected by mouse assay.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.75-83
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• 2017

The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.129-135
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• 2022

The official analytical method for the analysis of harmful heavy metals in Meju, distributed in Korea, employs a strong acid to decompose the organic components. This analysis is time consuming and harmful to the users and/or the environment. This study aimed to develop a new pre-treatment technology using laser ablation, to rapidly analyze harmful heavy metals without using strong acids. The results obtained from this method were validated by the National Institute of Food and Drug Safety Evaluation guideline (NIFDS, 2016). Moreover, a comparison of the two methods showed that the analytical time for 55 Meju samples was shortened by 96% or more in the new method. The results showed no significant difference in the recovery ranging from 90-120%. The proposed method proved suitable for detecting harmful heavy metals in Meju.

• Analytical Science and Technology
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• v.31 no.4
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• pp.143-148
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• 2018

Currently, the Korean Pharmacopoeia (KP XI) recommends HPLC and potentiometric titration (which is less specific than HPLC) for the determination of triflusal content in capsules and raw materials, respectively. Additionally, the British Pharmacopoeia (BP 2017) and European Pharmacopoeia (EP 8.0), which include a monograph for triflusal in raw materials only, describe a titration method for the assay. The latest version of the United States Pharmacopoeia (USP 39) and Japanese Pharmacopoeia (JP 17) still have not published monographs for triflusal and its preparations. To improve the specificity and efficacy of the assay, we present an HPLC method to determine triflusal content in both raw materials and capsules. The proposed method was validated in accordance with the requirements of the International Conference on Harmonization. A good linear relationship was achieved for triflusal in the range of $200-1250{\mu}g/mL$ with a coefficient of determination of approximately 0.9996. The relative standard deviations (RSDs) of inter- and intraday precision were 0.73-1.12 % and 0.34-0.51 %, respectively. The recovery percentage of triflusal was in the range of 98.80-101.31 %. Because its system suitability, intermediate precision, and robustness were satisfactory, this method could be suitable for determining triflusal content in raw materials and capsules.

• Analytical Science and Technology
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• v.31 no.3
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• pp.107-111
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• 2018

Currently, ultraviolet-visible spectrophotometry and titration methods are used for assay tests of tramadol hydrochloride injection and raw material in the Korean Pharmacopoeia XI (KP XI). Titration has also been used in the British Pharmacopoeia (BP 2013) for the assay test of tramadol hydrochloride, and the HPLC assay for tramadol hydrochloride raw material has been used in the United States Pharmacopeia (USP 39). In this study, we developed an alternative HPLC assay method for tramadol hydrochloride injection that is up to date and specific, and employs the same method as tramadol hydrochloride capsules. Validation of the HPLC method was conducted to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of the calibration curves in the desired concentration range was good ($r^2$ > 0.9999). RSDs of intra-day precision obtained were 0.05-0.08 % and inter-day precision obtained were 0.08-0.19 %. Accuracy was obtained with recoveries in the range of 98.16 % and 100.90 %. As a result of the system's suitability, the RSD of both retention time and the peak area obtained were 0.07 %. The values of the plate number and tailing factor of tramadol hydrochloride obtained were 7076 and 1.16, respectively. Because of the intermediate precision and robustness of the developed assay, it is expected to become a valuable tool for revising the Korean Pharmacopoeia (KP XI).

• Analytical Science and Technology
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• v.29 no.6
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• pp.277-282
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• 2016

British Pharmacopoeia (BP 2013), the United States Pharmacopoeia (USP 39) and the Korean Pharmacopoeia (KP XI) contain monographs for the quality control of raw diosmin using high performance liquid chromatography (HPLC). However, official monographs detailing pharmaceutical formulations for diosmin are not available in foreign pharmacopoeias. In the KP XI, ultraviolet-visible (UV-Vis) spectroscopy-which is less specific than HPLC-is reported for the testing of diosmin capsules. In this study, we present an alternative HPLC assay for such testing that is more specific than UV-Vis methods. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2$>0.999), while the RSDs for intra- and inter-day precision were 0.15-0.29 % and 1.05-1.74%, respectively. Accuracies ranged from 101.2-103.2 %, while the retention time and peak area RSDs were 0.37 % and 0.06 %, respectively. Additionally, the plate number and asymmetry factor values for diosmin were 3591.293 and 1.35, respectively. Since the intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

• Analytical Science and Technology
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• v.25 no.2
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• pp.91-101
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• 2012

A list of volatile fatty acids (VFA) including propionic acid, butyric acid, isovaleric acid, valeric acid, etc. is well known for offensive odorants. The analysis of odorant VFA is a highly delicate task due to high reactivity and unstable recovery rate. At present, analytical methods of VFA are recommended to include alkali impregnation filter method and alkali absorption method by the malodor prevention law of the Korea Ministry of Environment (KMOE). In this review, a survey has been made to explore various approaches available for the analysis of VFA to include both official methods of the KMOE and others. In light of the unreliability of those established analytical methods, it is highly desirable to develop some substituting methods for VFA. Among such options, one may consider such option as sorbent tube (ST) sampling and cryogenic trapping-thermal desorption technique. Moreover, procedures used for standard preparation, sampling steps, and instrumental detection stage are also evaluated. Application of container sampling (like Tedlar bag) is however not recommendable due to significant (sorptive) loss in sampling and in storage stage. In the detection stage, the use of GC/MS is recommendable to replace GC/FID due to the presence of diverse interfering substances. Thus, it is essential to properly establish the basic quality assurance (QA) for VFA analysis in air.

• Journal of Soil and Groundwater Environment
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• v.17 no.6
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• pp.33-42
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• 2012

This study was performed to find the problems according to interference factors (organic matter, pH, Cr, Mn, Fe, clay, and etc.) when we analyzed the hexavalent chromium [Cr(VI)] in soils using UV/VIS spectrometer (US EPA 7196A), attempted to evaluate the domestic applicability of analytical method (US EPA 7199) using IC-UV/VIS spectrometer as alternative method. The recovery rate of certified reference materials was 75.0% (US EPA 7196A) and 101.4% (US EPA 7199) by the analytical methods. As the results of performing QA/QC about US EPA 7199, method detection limit (MDL) and limit of quantification (LOQ) were 0.062 mg/kg, 0.196 mg/kg, respectively. The LOQ of US EPA 7199 was lower than that of the current soil official testing method in Korea (0.5 mg/kg). Cr(VI) contents in 23 soil samples were compared by the analytical methods of EPA 7196A and 7199. Cr(VI) was detected in 13 of 23 soil samples by EPA 7196A, while EPA 7199 was not detected in any soil samples. The Cr(VI) content in 23 soil samples by EPA 7196A was not clearly correlated with Cr, Fe, Mn and clay content in the soil samples. However, the contents of Cr(VI) and organic matter of the soil samples had the highest coefficient of determination ($R^2$) of 0.80. In order to evaluate the correlation between the recovery rates of Cr(VI) and organic matter contents in the soil samples, the recovery rates of 5 soil samples added Cr(VI) standard solution were analyzed by the analytical methods. According to the results, the higher the organic matter contents in soil samples, the lower the recovery rates of Cr(VI) by US EPA 7196, while in case of US EPA 7199, the recovery rates were stable regardless of the organic matter contents.

• The Korean Journal of Pesticide Science
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• v.18 no.2
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• pp.69-78
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• 2014

In the present study, we developed an official individual analytical method for cymoxanil using HPLC/UVD, respectively in different representative crops. Individual analytical methods for these pesticides are not included in the Korea food code. The samples were extracted with acetonitrile, concentrated and partitioned with dichloromethane and saturated sodium chloride solution. For cymoxanil, extracts were concentrated and clean-up through silica gel column chromatography with dicloromethane/acetone (60/40 v/v) and subjected to instrumental analysis. The limit of detection (LOD) for cymoxanil were 0.1 ng and 1 ng respectively and limit of quantitation (LOQ) were 0.02 mg/kg. Recoveries for cymoxail ranged from 79.6~107.6% respectively, at fortification level of 0.02 mg/kg (LOQ), 0.2 mg/kg (10 LOQ) and 1.0 mg/kg (50 LOQ) and the coefficient of variation (CV) was less than 10%, regardless of sample types. These results were further confirmed with LC/MS. The proposed simultaneous analysis method is reproducible and sensitive enough to determine the residues of cymoxanil in the agricultural commodities. According to the validation data and performance characteristics and high sample throughput, the proposed method is suitable for routine application.