• CELLMED
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• v.11 no.3
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• pp.13.1-13.9
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• 2021

Background and Objective: Nux-vomica based traditional Unani formulation, Habb-e-Azaraqi (HAZ) is an important drug used by Unani physicians since several decades. It possesses Muqawwi-i-A'sab (nervine tonic), Muharrik-i-A'sab (nervine stimulant) properties and is an effective treatment option for diseases like Laqwa (facial palsy), Falij (paralysis), Niqris (gout) and Waja'al-Mafasil (arthritis) etc. The aim of the study is to access and provide information of HAZ for its TLC, HPTLC Fingerprinting defining its clear qualitative perspective and acute oral toxicity evaluation for its safety assessment which was not done earlier, thus contributing in the field of research. Materials and Methods: The chief ingredient, nux-vomica was detoxified as per method mentioned in Unani Pharmacopeia before its use in formulation. TLC and HPTLC was developed under four detection system i.e., UV 366nm, UV 254nm, exposure to iodine vapours and after derivatization with anisaldehyde sulphuric acid. Acute toxicity studies were performed as per OECD Guidelines 425 at a limit dose of 2000 mg/kg. Observations were done for signs of toxicity, body weight, and feed consumption at regular intervals followed by haematological and biochemistry evaluation. Results: The generated data proved the authenticity and established the TLC and HPTLC profile of the formulation. Acute toxicity revealed no significant differences in HAZ-treated animals with respect to body weight gain, feed consumption, haematology, clinical biochemistry evaluation. No significant gross pathological observation was noticed in necropsy. Conclusion: Data of the present study is substantial and scientific proof of HAZ in terms of standardization and toxicity study that can be utilize in future research activities.

• Analytical Science and Technology
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• v.19 no.2
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• pp.142-148
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• 2006

To determine malachite green and leuco-malachite green residues in sea food, a liquid chromatographic method has been optimized. The target compounds were extracted in the homogenized edible tissues with a mixture of McIlvaine buffer-acetonitrile and partitioned against dichloromethane. After concentrating the lower layer, the resulting residues were re-dissolved in methanol and analyzed by the HPLC with visible detector at 620 nm using acetonitrile-acetate buffer. For the analysis of leuco-malachite green with malachite green simultaneously, post-column packed with lead(IV) oxide was used for oxidizing leuco-malachite green to malachite green. The correlation coefficients($r^2$) was 0.9989 for malachite green, and 0.9995 for leuco-malachite green. The limit of detection was 0.005 mg/kg for the combined of malachite green and leuco-malachite green at signal/noise${\geq}3$. The recovery rate was within a reliable range of 84~98% (CV 3~16%). Leuco-malachite green were detected in carp and crusian carp.

• Analytical Science and Technology
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• v.19 no.5
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• pp.383-388
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• 2006

Simple post-wash method by ion chromatography (IC) was established for the rapid and precise determination of fluoride ion in wastewater from mine in fluorite mineralized area. High sulfate in sample was retained in a pre-column and less strongly held fluoride ion was transferred to the principal separation system using modified conventional IC with switching technique. An analytical column with high capacity (AS 9 HC) was used as a pre-column to retain the amount of high sulfate. A guard column (AG 14) as a separation column was used to increase the response of fluoride and reduce the system pressure. According to the recovery of fluoride ion with one detector and the observation of sulfate peak with another conductivity detector, the optimum switching time of 10-port chromatographic injector was 4.3 min. The limit of detection (S/N = 3) of fluoride in synthetic solution containing $500mg\;L^{-1}$ sulfate was $2.4{\mu}g/L$, with $25{\mu}L$ sample volume.

• Analytical Science and Technology
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• v.20 no.1
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• pp.84-90
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• 2007

To determine levels of 11 sulfonamides for animals in food, simultaneously, a selective method of high performance liquid chromatography with UV detector has been applied. The targets were sulfachlorpyridazine (SCP), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfisoxazole (SSX), sulfamerazine (SMZ), sulfamethazine (SMT), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfaquinoxaline (SQX) and sulfathiazole (STZ). Food samples were beef, pork, chicken, milk and whole egg that were collected at the main 6 cities in Korea as Seoul, Busan, Daejon, Incheon, Mokpo and Gangneung. After homogenizing food samples with sodium phosphate solution and acetonitrile, it was extracted with n-hexane. The mobile phase gradient was a mixture of 5 mM potassium phosphate (pH 3.25) and methanol with a gradient ratio from 100:0 to 30:70. The UV wavelength was 270 nm. The overall recoveries were ranged from 75% to 95% and the limit of detection was minimum 0.004 mg/kg for SMT, and 0.007 mg/kg for STZ at signal/noise > 3, respectively. As results, sulfonamide drugs were not detected in most of the selected food samples, however, sulfamonomethoxine was detected in meat. The determined level of sulfamonomethoxine were 0.03 and 0.06 mg/kg for beef that were below the MRLs.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.128-133
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• 2024

Using the freezing removal method, we investigated residual pesticides in 50 grape seed oils distributed in Gyeonggi Province, South Korea. The fat was mixed with acetonitrile and then frozen at ≤-20℃ for 24 h. Fats and oils were removed by separating those in solid state and the extract acetonitrile in liquid state. Ten residual pesticides were detected 161 times in 49 of 50 cases. The detected pesticides were boscalid, cyclufenamide, deltamethrin, difenoconazole, fluxapyroxad, fenpyrazamine, kresoxim-methyl, piperonyl butoxide, tebuconazole, and trifluoxysorbin. Boscalid, a fungicide, was most frequently detected (44 times), followed by fluxapiroxad (35 times). The detection range was 0.01-1.10 mg/kg, which was within the legal limit of residual pesticide for grapes. The recovery rate of the detected pesticides was 72.6-129.8% and the ratio of estimated daily intake/acceptable daily intake was calculated to determine the risk of the detected pesticides, which was <0.0028%. This indicated that the risk caused by pesticide residues in grape seed oil is at a safe level.

• Analytical Science and Technology
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• v.27 no.5
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• pp.234-242
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• 2014

Imicyafos which is a nematicide for controlling root-knot nematodes has been registered in the Republic of Korea in 2012, and the maximum residue limits of imicyafos are set to watermelon and korean melon as each 0.05 mg/kg. Extremely reliable and sensitive analytical method is required for ensuring food safety on imicyafos residues in agricultural commodities. Imicyafos residues in samples were extracted with acetone, partitioned with hexane and dichloromethane, and then purified with florisil. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. Linear range was between 0.1~5 mg/kg with the correlation coefficient ($r^2$) 0.99997. Average recoveries of imicyafos ranged from 77.0 to 115.4% at the spiked levels of 0.02 and 0.05 mg/kg with the relative standard deviations of 2.2~9.6%. Limit of detection and quantification were 0.005 and 0.02 mg/kg, respectively. An inter-laboratory study was conducted to validate the determination method in depth, and the results were satisfactory. All of the validation results revealed that the developed analytical method in this study is relevant for imicyafos determination in agricultural commodities and will be used as an official analytical method.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

• Korean Journal of Food Science and Technology
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• v.43 no.2
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• pp.125-133
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• 2011

The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

• Korean Journal of Food Science and Technology
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• v.45 no.4
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• pp.391-402
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• 2013

Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.

• Journal of Food Hygiene and Safety
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• v.35 no.1
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• pp.23-30
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• 2020

This study investigated the migration levels of lead (Pb), cadmium (Cd), and arsenic (As) from food contact articles (glassware, ceramics, enamelware, and earthenware) into a food stimulant (4% v/v, acetic acid). Migration tests were performed at 25℃ for 24 h and all analyses were performed using Inductively-Coupled Plasma Mass Spectrometry (ICP-MS). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision, and uncertainty. In glassware, the migration concentrations ranged from not-detected (N.D.) to 752.21 ㎍/L and N.D. to 1.99 ㎍/L for Pb and Cd, respectively. In ceramics, the migration concentrations ranged from N.D. to 1,955.86 ㎍/L, N.D. to 74.06 ㎍/L, and N.D. to 302.40 ㎍/L for Pb, Cd, and As, respectively. In enamelware, the migration concentrations ranged from N.D. to 4.48 ㎍/L, N.D. to 7.00 ㎍/L, and N.D. to 52.00 ㎍/L for Pb, Cd, and Sb, respectively. In earthenware, the migration concentrations ranged from N.D. to 13.68 ㎍/L, N.D. to 0.04 ㎍/L, and N.D. to 6.71 ㎍/L for Pb, Cd, and As, respectively. All results were below the migration limits of Korea standards and specifications for food utensils, containers, and packages.