• Journal of Physiology & Pathology in Korean Medicine
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• v.32 no.5
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• pp.333-340
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• 2018

Gamiguibi-tang (GGBT) is a traditional herbal medicine generally used to treat anemia, insomnia, anxiety, and nervousness. GGBT is being commercially produced in the form of extract granule and the quality control methods are specified in the Korean Herbal Pharmacopeia (KHP). However, there is no method to simultaneously analyze compound preparations. In this study, a HPLC method was developed and validated for the simultaneous determination of marker compounds in GGBT. And the contents of marker components and biological activities of the commercial GGBT extract granules (GGBT-2 and GGBT-3) were compared with those of the GGBT decoction (GGBT-1). We confirmed the robustness of simultaneous analytical method by monitoring the contents of the commercial GGBT products and carrying out validation. The marker components of GGBT were geniposide ($8.03{\sim}12.70{\mu}g/mL$), paeoniflorin ($2.79{\sim}4.25{\mu}g/mL$) and glycyrrhizic acid ($5.06{\sim}6.30{\mu}g/mL$). DPPH and ABTS radical scavenging activities were 47.34~63.17% and 21.52~33.61% in the GGBT products concentration of $1,000{\mu}g/mL$, respectively. The GGBT products significantly decreased NO, iNOS and COX-2 production in lipopolysaccharide (LPS)-induced RAW 264.7 macrophages in a concentration-dependent manner. The GGBT-2 had higher contents of marker components and biological activities than GGBT-1 and GGBT-3. The research suggest that be used in developing quality control methods for enhancing the quality of herbal medicines.

• Korean Journal of Environmental Agriculture
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• v.39 no.4
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• pp.368-374
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• 2020

BACKGROUND: The residual analysis of polar pesticides has remained a challenge. It is even more difficult to simultaneously analyze multiple polar pesticides. Diquat, paraquat, and chlormequat are typical examples of highly polar pesticides. The existing methods for the analysis of diquat, paraquat and chlormequat are complex and time consuming. Therefore, a simple, quick and effective method was developed in the represent study for simultaneous analysis of diquat, paraquat and chlormequat in animal products, meat and fat using UPLC-MS/MS. METHODS AND RESULTS: Sample extraction was carried out using acidified acetonitrile and water and re- extracted with acidified acetonitrile and combine the extracts followed by centrifugation. The extract was then cleaned up with a HLB cartridge after reconstitution with acidic acetonitrile and water. The method was validated in quintuplicate at three different concentrations. The limits of detection (LOD) and quantification (LOQ) were 0.0015 and 0.005 mg/L, respectively. Matrix suppression effect was observed for all of the analytes. A seven point matrix matched calibration curve was constructed for each of the compound resulted excellent linearity with determination coefficients (R2) ≥ 0.991. Accuracy and precision of the method was calculated from the recovery and repeatability and ranged from 62.4 to 119.7% with relative standard deviation less than 18.8%. CONCLUSION: The recovery and repeatability of the developed method were in the acceptable range according to the Codex Alimentarius guideline. The developed method can be applied for the routine monitoring of diquat, paraquat, and chlormequat in animal products, meat and fat.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.36 no.3
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• pp.167-174
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• 2010

The hair nourisher products are used for prevention of hair loss and classified as quasi-drug in Korea. As concerns about hair loss has been increased, the demand for hair nourisher products has been growing. It is difficult to analyze their main ingredients because they contain various ingredients including natural plant extracts, vitamins, preservatives and exfoliators. The purpose of this study was to develop and validate simultaneous analytical methods of active ingredients in hair nourisher products such as nicotinamide, tocopherol, salicylic acid, dexpanthenol and benzyl nicotinate by HPLC. The active ingredients were separated on a $C_{18}$ column by using acetonitrile/phosphate buffer as a mobile phase, and detected at UV 220, 270 and 300 nm. The calibration curve showed linearity in the range of $12.5{\sim}800\;{\mu}g/mL$ and the recoveries were 97.3 ~ 103.5 % (RSD 0.9 ~ 2.8 %) in liquid matrix and 101.9 ~ 115.9 % (RSD 0.7 ~ 7.7 %) in shampoo matrix. Validated method was applied to hair nourisher products obtained from distribution market. Fortunately, all samples met their criteria. This study might be expected to provide the method for determining active ingredients in hair nourisher products and lead to promote a rapid market entry.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.130-137
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• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

• Journal of the Korean Chemical Society
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• v.38 no.6
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• pp.418-426
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• 1994

This study was aimed at the detection of 40 semi-volatile organic base/neutral compounds from soil among 129 priority pollutants listed by EPA. Two extraction procedures, sonication extraction and Soxhlet extraction, were studied as a extraction and concentration method for priority pollutants in soil. Extracts were analyted by GC/MS-SIM(selected ion monitoring). The analytical methods were tested by standard compounds spiked into blank soil. Accuracy and precision of the methods were measured by calculation of mean recovery and mean relative standard deviation. And the method detection limits were estimated.

• Applied Biological Chemistry
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• v.40 no.2
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• pp.144-147
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• 1997

Different isolation methods for the volatile components of Anise(Pimpinella anisum L.) are compared in terms of the difference of components obtained with each analytical procedure. These methods include headspace(purge & trap) sampling procedure, simultaneous distillation extraction(SDE), steam distillation and solvent extraction. Total 43 components were identified by? comparing gas chromatography retention time and mass spectral data. Different isolation techniques result in compositionally different isolates. The headspace(purge & trap) sampling procedure was found to be the best method of choice for a qualitative analysis of the volatile components.

• Korean Journal of Environmental Agriculture
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• v.42 no.3
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• pp.220-230
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• 2023

Imidacloprid is a neonicotinoid insecticide widely used for insect control in a variety of crops. The evaluation of imidacloprid total residues in animal feeds derived from crop by-products is required to ensure the safety of livestock products. We performed simultaneous LC/MS/MS analyses of imidacloprid and its metabolites in five different livestock products including beef, pork, chicken, milk and egg from domestic markets. The methods for sample preparation and instrumental analysis were established by modifying QuEChERS method to meet the Codex guidelines. The methods generated 0.0035 mg/kg of the limit of determination (LOD), 0.01 mg/kg of the limit of quantitation (LOQ) and standard calibration linearity with >0.983 of the coefficients of determination (R²). The methods exhibited the recovery values of imidacloprid and its metabolites ranging from 65.66 to 119.27% without any interference between matrices. Imidacloprid total residues in the livestock products were found as values lower than the LOQ and maximum residue limits (MRLs). This study suggests that the methods are successfully applicable for the safety evaluation of imidacloprid total residues in livestock products from domestic markets.

• Analytical Science and Technology
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• v.33 no.3
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• pp.125-133
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• 2020

Methylisothiazolinone (MIT) and chloromethylisothiazolinone (CMIT) cause allergic contact dermatitis and are banned cosmetics ingredients, except in rinse-off products. However, their presence has been detected in cosmetics. We report a UPLC-tandem MS/MS screening method for their simultaneous determination in cosmetics. To facilitate extraction from various matrices, pretreatment methods were developed for each sample type. The method was optimized through a series of assessments, including specificity, LOD, LOQ, linearity, recovery, stability, precision, and accuracy. The LODs and LOQs for MIT ranged from 0.054 and 0.163 ㎍ mL^-1 whereas those for CMIT ranged from 0.040 and 0.119 ㎍ mL^-1. The linear correlation coefficients (r²) were higher than 0.999. Relative standard deviations (RSDs) for both intra- and inter-day measurements ranged from 0.3 ~ 13.6 %. Recoveries at three different concentrations were within 87.9 ~ 118.9 %. The RSD for stability measurements of spiked samples was within 7 %. These results confirm the suitability of the developed method for the simultaneous quantitation of MIT and CMIT in cosmetics. Samples of 320 color cosmetics, including eyeshadows, solid lipsticks, liquid lipsticks, and nail polishes were analyzed using the developed method, and two of them were found to contain both MIT and CMIT and one of them was found to contain only MIT. This data and the method will aid the regulation of ingredients used in cosmetics.

• Journal of the Korean Chemical Society
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• v.46 no.5
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• pp.419-437
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• 2002

An analytical method for the spectrometric simultaneous determination of the individual ions in the mix-tures of $Fe^{2+}$ and $Fe^{2+}$ ions utilizing a technique of flow injection analysis has been developed. The method was based on the oxidation reaction between $Fe^{2+}$ ion and $H_2O_2$ in an acidic medium and the subsequent formation of a red Fe$(SCN)^{3-x}_x$ ion by the complexation reaction between $Fe^{2+}$ ion and $SCN^-$ ion. Unlike the conventional methods which require separate processes for the pre-treatment of the sample solution, the current method uses the same FIA system for the pre-treatment and the analysis of the sample. The detection limit for the determination of $Fe^{2+}$ ion was found to be 6.00${\times}10^{-7}$M.

• Journal of the Korean Chemical Society
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• v.33 no.1
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• pp.46-54
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• 1989

The extraction method and quantitative analysis for the fat-soluble vitamins present in food stuffs and vitamin products have been investigated. The simultaneous separation and analysis of the vitamins by reverse phase high performance liquid chromatographic method was conducted using an isocratic elution with methanol : water (95 : 5) eluent on a Novapak $C_{18}$ column. The detection of vitamins was achieved by a variable wavelength UV detector. To improve the detection sensitivity detection wavelengths were set at the highest absorption bands such as 330, 265, 285, and 290nm for the respective vitamins. The analysis for the fat-soluble vitamins was finished within 40 minutes. Alkaline hydrolysis and enzymatic hydrolysis were investigated for the sample preparation; and liquid-liquid extraction and liquid-solid extraction were attempted for the extraction of vitamins. Both hydrolysis methods were turned out to be appropriate for the analysis for vitamins A, D, and E, while for the analysis of vitamin K the enzymatic hydrolysis method demonstrated better results. Diethyl ether, pentane, and n-hexane were found to give higher recovery for the liquid-liquid extraction and silica cartridge for the liquid-solid extraction.