• Toxicological Research
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• 제26권2호
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• pp.149-155
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• 2010

The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

• 약학회지
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• 제58권3호
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• pp.190-199
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• 2014

The Korean Pharmaceutical Codex (KPC) analytical method of ambroxol hydrochloride and clenbuterol hydrochloride formulation is complicated and needed to carry out multiple processes during the test. To improve the low efficiency of analytical procedure that makes pharmaceutical laboratory consume much time and high cost to conduct the test of this formulation, this study was performed for simplifying the pretreatment process and optimizing conditions of the HPLC assay. The analytical procedure using HPLC was developed to establish analytical specification for ambroxol hydrochloride and clenbuterol hydrochloride formulations. The newly developed analytical method has good linearity ($R^2$ >0.999), specificity, precision (RSD<1.0%) and the recovery ranges of 98.50~101.84% for ambroxol, 98.29~101.35% for clenbuterol syrup and 98.66~101.71% for clenbuterol tablets. The LOQs were 0.204 ${\mu}g/ml$ for ambroxol, 0.021 ${\mu}g/ml$ for clenbuterol syrup and 0.073 ${\mu}g/ml$ for clenbuterol tablets. The new method was performed with commercially available samples to confirm analytical conditions and validated to be suitable for saving time and cost to control the quality of routine manufactured products. This analytical method will be used for revising the monograph of ambroxol hydrochloride and clenbuterol hydrochloride formulation in next supplement of KPC.

• 한국환경농학회지
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• 제40권2호
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• pp.127-133
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• 2021

BACKGROUND: Dithiocarbamte fungicides have been used in crop cultivation for diseases protection and treatment. And cultivated agricultrual products were used as feedstuff, and residual pesticides are likely to be absorbed and transferred to livestock. But the maximum residue limits (MRLs) were not established for dithiocarbate fungicides in livestock products, and thus an analysis method was developed and validated for dithiocarbamate fungicides to establish MRLs. METHODS AND RESULTS: Samples were prepared using CS₂ trap method and detected with UV/VIS spectrophotometer. Calibration line (0.1 ~ 10 ㎍/mL) was linear with r² > 0.99. For validation, the recovery tests were carried out at three fortification levels (MLOQ, 10 MLOQ and 50 MLOQ) from livestock samples (egg, milk, beef, pork, and chicken). The results for mancozeb, propineb, and thiram ranged between 76.8 to 109.6%, 79.4 to 108.8%, and 80.2 to 107.8%, respectively and % RSD (relative standard deviation) values were below 9.5%. Furthermore, inter-laboratory analysis was performed 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). This might be used as an official analytical method for determination of dithiocarbamate fungicides at established MRLs and monitoring.

• 한국환경농학회지
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• 제40권2호
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• pp.99-107
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• 2021

BACKGROUND: Pesticide uptake by a rotational crop after being used for the primary crop is a potential cause of violation against the pesticide law if the pesticide is not registered in the secondary crop. This study was conducted to investigate the plant back interval (PBI) of fluopyram for the rotational cultivation of radish. METHODS AND RESULTS: Two experimental approaches were performed the evaluation of residues in radish cultivated successively in soil 16 days after treated with fluopyram onto pepper plant (T1) and in radish cultivated in bare soil treated with fluopyram at PBI 30 and PBI 60 days (T2). A modified QuEChERS method coupled with LC/MS/MS analysis showed good linearity of matrix-matched standard calibration of fluopyram with the coefficient values of determination greater than 0.995. Recovery values at levels of 0.01, 0.05, 0.1 and 0.25 mg/kg ranged from average 84.9 to 117.6% with RSD less than 10%. Fluopyram residues in radish harvested from T1 and T2 were found as levels less than maximum residue limit. CONCLUSION: This study suggests 20~30 days as the PBI of fluopyram for the rotational cultivation of radish in the greenhouse soil treated with fluopyram used for pepper as the primary crop.

• 분석과학
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• 제32권4호
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• pp.139-146
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• 2019

A simple and reliable analytical method based on high-performance liquid chromatography-ultraviolet detection was established for the analysis of the flowers of Chrysanthemum morifolium (CM). Luteolin-7-O-glucoside (LU7G) was chosen as a target analyte considering its content, availability, and ease of analysis. Chromatographic separation of LU7G was achieved using a Phenomenex Gemini $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) run with a mobile phase consisting of 0.5 % acetic acid in water and 0.5 % acetic acid in acetonitrile at a flow rate of $1.0mL\;min^{-1}$. The detection wavelength and column temperature were set at 350 nm and $40^{\circ}C$, respectively. Method validation was performed according to the AOAC guidelines and the method was specific, linear ($R^2=0.9991$ for $50-300{\mu}g\;mL^{-1}$), precise (${\leq}3.91%$RSD), and accurate (100.1-105.7 %). The limits of detection and quantification were 3.62 and $10.96{\mu}g\;mL^{-1}$, respectively. The established method was successfully applied to determine the contents of LU7G in various batches of bulk CM extracts and labscale CM extract. The developed method is a readily applicable method for the quality assessment of CM and its related products.

• 분석과학
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• 제32권4호
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• pp.147-154
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• 2019

Ampicillin and Sulbactam (2:1, w/w) are combined in formulation to provide broader antibacterial action in treatment of many infections. The development of analytical method for simultaneouly determine these two compounds was difficult because of the differences in their chemical structures and ratio in the formulation. Current published methods still have some limitations. In this study, we developed an alternative high-performance liquid chromatography (HPLC) assay method for simultaneously determination of ampicillin sodium and sulbactam sodium in powder for injection. Method validation of HPLC method was conducted to determine linearity, precision, accuracy, system suitability, robustness. The linearity of the calibration curves in the desired concentration range was good ($r^2$> 0.9994). RSDs of intra-day and inter-day precision obtained were less than 2.00 %. Accuracy was obtained with the recoveries in range of 98.42 % and 101.36 %. As a result of system suitability, RSD of both retention time and the peak area obtained were not more than 1.0 %. The values of plate number were more than 7000 and symmetric factors obtained were 0.8. As intermediate-precision and robustness of the developed assay, it could be expected to become valuable tools for revising the Korean Pharmacopoeia (KP XI).

• 생약학회지
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• 제52권3호
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• pp.186-191
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• 2021

We developed a method to identify and quantify 6-hydroxyluteolin 7-O-glucoside in the powder of Salvia plebeia (PS) using high-performance liquid chromatography coupled with diode array detector (HPLC/DAD) and equipped with reverse-phase INNO C18 column. The analytical method was optimized and validated using novel parameters. The obtained values for the limits of detection and quantification were 3.60 and 10.90 ㎍/mL, respectively. Calibration curve showed good linearity in the concentration range tested (0.00625-0.1 mg/mL, r² = 1.0000), high accuracy (96.2-101.4%), and precision values (RSD ≤ 0.27%). Our analysis support the use of our method for accurately identifying and quantifying 6-hydroxyluteolin 7-O-glucoside from PS in routine analyses and large-scale extraction processes for content determination.

• Natural Product Sciences
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• 제27권2호
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• pp.128-133
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• 2021

The Coumarin (1,2-benzopyrone) is the main secondary metabolite of Mikania laevigata Sch. Beep ex Baker and Mikania glomerata Spreng., which are popularly known as guaco. These plants have been used mainly in traditional medicine in the treatment of respiratory diseases because their bronchodilator effect. However, there are around 200 species of Mikania, which are quite similar in appearance. From these, only M. leavigata and M. glomerata have high concentrations of coumarins. In this line, the falsification of products Mikania based has been frequent. In this sense, this work demonstrated the application of the easy, fast, e not destructive method based in Nuclear Magnetic Resonance in quantitative mode (qNMR) for the determination of coumarin in both commercial and homemade guaco products. Thus, in the first step the compounds were extract from guaco leaves and syrups using chloroform (CHCl₃), with or without ultrasound. About the method, was linear with a R² = 0.9947 for 1,2-benzopyrone, with detection and quantification limits with were 0.11 and 0.36 mg mL^-1 respectively. In the same line, the method was safe with RSD <0.3% and with recovery ranging from 93-101%. To confirm the applicability of the method, in the last step was applied to 10 real samples (6 from leaves and 4 from syrups). The content of the coumarin in the leaf extract ranged from 0.62 to 1.30 mg mL^-1. For syrups I, II and IV, the content of coumarin was in accordance with the manufacturers. However, for de Syrup III, the concentration was 155% higher. In summary, the qNMR is a rapid method with minimal sample preparation that can be used to quantify coumarin in home-made plant extracts as well as in commercial samples as syrup for instance. This method is applicable for quality control of different plants-based products.

• Advances in nano research
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• 제10권3호
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• pp.295-312
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• 2021

A new ionic liquid functionalized magnetic silica nanoparticle was synthesized and characterized and tested as an adsorbent. The adsorbent was used for magnetic solid phase extraction on ICP-MS method. Simultaneous determination of precious metal Au has been addressed. The method is simple and fast and has been applied to standard water and surface water analysis. A new method for separation/analysis of trace precious metal Au by Magnetron Solid Phase Extraction (MSPE) combined with ICP-MS. The element to be tested is rapidly adsorbed on CoFe2O4@SiO2@[BMIM]PF6 composite nano-adsorbent and eluted with thiourea. The method has a preconcentration factor of 9.5-fold. This method has been successfully applied to the determination of gold in actual water samples. Hydrophobic Ionic Liquids (ILs) 1-butyl-3-methylimidazole hexafluorophosphate ([BMIM]PF6) coated CoFe2O4@SiO2 nanoparticles with core-shell structure to prepare magnetic solid phase extraction agent (CoFe2O4@SiO2@ILs) and establish a new method of MSPE coupled with inductively coupled plasma mass spectrometry for separation/analysis of trace gold. The results showed that trace gold was adsorbed rapidly by CoFe2O4@SiO2@[BMIM]PF6 and eluanted by thiourea. Under the optimal conditions, preconcentration factor of the proposed method was 9.5-fold. The linear range, detection limit, correlation coefficient (R) and relative standard deviation (RSD) were found to be 0.01~1000.00 ng·mL-1, 0.001 ng·mL-1, 0.9990 and 3.4% (n = 11, c = 4.5 ng·mL-1). The CoFe2O4@SiO2 nanoparticles could be used repeatedly for 8 times. This proposed method has been successfully applied to the determination of trace gold in water samples.

• 생약학회지
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• 제51권4호
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• pp.270-277
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• 2020

This study analyzed mycotoxins, aflatoxin B1, B2, G1, G2, fumonisin B1, B2, ochratoxin A and zearalenone, using LC-MS/MS and conducted risk assessment on 54 samples of seeds distributed in SeoulYangnyeongsi and the management status of extramural herbal dispensary facility. The matched calibration showed a good linearity as observed in 6 concentration levels(r2>0.999) as a result of method validation applied with Arecae semen. Limits of detection(LOD) and quantification(LOQ) were in the range of 0.02-0.11 ㎍/kg and 0.08-0.34 ㎍/kg, respectively. Recoveries also estimated, ranging from 65.1-99.7% with relative standard deviation(RSD) 0.5-6.3%. As a result of the method on 54 samples, mycotoxins were detected in 16 samples. Among them, two Thujae semen showed a degree of concentration that exceeded the aflatoxin specification. In the risk assessment, the human exposure safety standard values were calculated as ADI(Acceptable Daily Intake) for aflatoxin B1, fumonisin and zearalenone. Ochratoxin A was calculated as PTWI(Provisional Tolerable Weekly Intake). The MOE(Margine of Exposure) of aflatoxin B1 was in the range of 40.36-3536.88. And no items exceeded 100% in %TDI(Tolerable Daily Intake) and %TWI(Tolerable Weekly Intake) of fumonisin, zearalenone and ochratoxin A.