• Title/Summary/Keyword: GC/NPD

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A Study on Removal Effect of Residual Pesticide on Adsorbent (흡착제에 의한 잔류농약 제거효과에 관한 연구)

  • An, Jung-hyeok;Kim, Joon-bum;Kwon, Young-du;Jeon, Choong;Park, Kwang-ha
    • Applied Chemistry for Engineering
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    • v.18 no.6
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    • pp.537-544
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    • 2007
  • This study was carried out to investigate adsorption characteristics of residual pesticides on an adsorbent. $Bauxsol^{TM}$ and mackban-stone as adsorbent were used. Analytical method for residual pesticides was established by GC/NPD and $GC/{\mu}ECD$. Pesticides used in this study were ${\alpha}$-endosulfan, ${\beta}$-endosulfan, pendimethalin and chlorpyrifos-methyl, fenitrothion, and recovery rates were more than 97%. Adsorption rate on an adsorbent was decreased in order of endosulfan, chlorpyrifos-methyl, pendimethalin, fenitrothion. Organochlorine pesticides showed higher removal rate than the other pesticides. $Bauxsol^{TM}$ gave both chemical decomposition and physical adsorption. Mackban-stone gave only physical adsorption on the other hand. The high pH and chloric ions structure of eluted solution have greatly affected at chemical resolution. The removal rate of pesticides was increased due to the physical property of adsorbent, i.e. high porosity. The above adsorbent is to be a candidate to remove residual pesticides in water and pond of links.

Quantitative Analysis of Tiropramide in Human Blood by Gas Chromatography with Nitrogen-Phosphorus Detector

  • Kwon, Oh-Seung;Park, Young-Jin;Ryu, Jae-Chun;Chung, Youn-Bok
    • Archives of Pharmacal Research
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    • v.26 no.5
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    • pp.416-420
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    • 2003
  • The analytical method of antispasmodic agent tiropramide {$(\pm)\alpha$-(benzoylamino)-4-[2-(diethylamino)ethoxy]-N,N-dipropylbenzenepropanamide hydrochloride} was developed by gas chromatography/nitrogen-phosphorus detector (GC/NPD) in human plasma. Two kinds of tiropramide tablets were orally administered to volunteers by Latin square crossover design, and blood was withdrawn as designed schedule. The plasma of 1 mL was loaded on Sep-pak $C_{18}$ cartridge and eluted with methanol after washing with 30% methanol. The residue dissolved in 100 $\mu$L of methanol after evaporation was analyzed by GC/NPD. Precision (CV%) of intra-day was located within 2.6% and accuracy was less than 9.7%. Inter-day precision was below 8.7% and accuracy was relatively good as less than 14%. Plasma samples obtained from human volunteers were analyzed for the determination of tiropramide concentration by using this method. The method was sensitive, rapid and suitable enough to be applied for pharmacokinetic and bioequivalence studies of tiropramide in human volunteers.

Residual Pesticides in Dried Agricultural Products Collected from Gyeonggi Province (경기도내 유통 건조농산물의 잔류농약 실태)

  • Lee, Myung-Jin;Kim, Myung-Gil;Jeong, Hong-Rae;Yun, Hee-Jeong;Kim, Nan-Young;Kim, Han-Taek;Kim, Chol-Young;Lee, Woon-Hyung;Yoon, Mi-Hye
    • The Korean Journal of Pesticide Science
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    • v.15 no.3
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    • pp.238-245
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    • 2011
  • This study was carried out to examine residual pesticides in dried agricultural products collected from Gyeonggi province in 2010. A total of 102 samples was collected and analyzed for 206 pesticides by multiresidue method using GC-${\mu}ECD$, GC-NPD, GC/TOF/MSD, HPLC-UVD, HPLC-FLD and HPLC/MS/MS. The detection rate of residual pesticides was 23.5% (24 of 102 samples) and the agricultural products exceeding their MRLs (Maximum Residue Limits) were 1 sample of pepper leaves. Additionally, the frequently detected pesticide were chlorothalonil, fenvalerate, chlorpyrifos, endosulfan, bifenthrin, cypermethrin, hexaconazole and iprodione. The pesticide types detected in the dried agricultural products showed in the descending order of organophosphorus (22%), pyrethroid (22%), organochloride (17%), dicarboxymide (11%), carboxymide (6%), carbamate (6%), triazole (5%) and the others (11%).

Monitoring and risk assessment of pesticide in school foodservice products in seoul, Korea (서울지역 학교급식 식재료의 잔류농약 위해성 평가)

  • Seo, Young-Ho;Moon, Kwang-Deog
    • Food Science and Preservation
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    • v.21 no.1
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    • pp.69-74
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    • 2014
  • We tested for residual pesticide levels in school foodservice agricultural products in Seoul, Korea from 2010 to 2012. A total of 316 samples of 23 different types of agricultural products were analyzed via gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography-ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze 185 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 26 samples (8.2%), of which 6 samples (1.9%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in more than 65% of the Chwinamul, while 6 among 9 analyzed samples contained pesticide residue, and 1 sample exceeded the Korea MRLs. Among the 185 kinds of pesticides that we have tested, 18 were detected, while 7 of them were detected more than twice. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The most critical commodity is carbofuran in the perilla leaves, which has contributed 3.8% to the hazard index (HI). These results showed that the detected pesticides could not be considered as a serious public health problem. Nevertheless, constant supervision is recommended.

A Study on the Safety of Residual Pesticides in Cereal Grains and Pulses Agricultural Products Excluding Rice (잡곡 농산물의 잔류농약 안전성 조사)

  • Han, Na-Eun;Kim, Jae-Gwan;Yun, Hee-Jeong;Kang, Min-Seong;Cho, Young-Seon;Song, Ji-Won;Kim, Byeong-Tae;Lee, Seong-Nam;Choi, Ok-Kyung
    • Journal of Food Hygiene and Safety
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    • v.37 no.1
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    • pp.1-8
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    • 2022
  • In this study, the pesticide residues in 106 commercial cereal grains were monitored from February to July 2021. For the investigation, 40 domestic and 66 imported products from large, small-to-medium sized offline and online distribution channels, were collected and analyzed by using the multiresidue method for 341 pesticides on GC/ECD, GC/NPD, GC/MSMS, UPLC/PDA, HPLC/FLD, LC/MSMS. Pesticides were detected in total of 8 samples (7.5%), of which one was from big box retailers, two from small and medium-sized distribution stores, and five from online shopping mall. Five (4.7%) samples were found to have pesticide residues greater than the maximum residue limits (MRLs). The detected pesticides in kidney beans (1 case), mung beans (6 cases), and sorghum (1 case), were MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, and pirimiphos-methyl. Specifically, an excessive amount of thiamethoxam was found from the imported mung bean (5 cases).

Analysis of Hexaconazole in Agricultural Products using Multi Class Pesticide Multiresidue Method (다종 농약 다성분 분석법을 이용한 농산물 중 hexaconzole 분석)

  • Choi, Su Jeong;Hwang, In Sook;Cho, Tae Hee;Lee, Jae In;Lee, In Sook;Yook, Dong Hyun;Park, Won Hee;Kim, Moo Sang;Kim, Gun Hee
    • Journal of Food Hygiene and Safety
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    • v.30 no.4
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    • pp.366-371
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    • 2015
  • This work was conducted to apply the multi class pesticide multiresidue method for determining the use of hexaconazole in the agricultural products using GC-NPD. The multi class pesticide multiresidue method results were validated for the assay of hexaconazole by using linearity, accuracy, precision, limit of detection and quantitation. The linearity in the concentration ranged from 0.025 to 5.0 mg/L ($R^2$ > 0.999). Lettuce recoveries ranged from 89.42% to 94.15% with relative standard deviations below 7.78%, for spiking levels from 0.04 to 4.0 mg/kg. The limit of detection was 0.04 mg/kg, and the limit of quantitation was 0.11 mg/kg. The intra- and inter-day precisions were 2.42~3.49% and 4.90~7.78%, respectively. We suggested that the multi class pesticide multiresidue method for determining hexaconazole was highly accurate and reproducible, and it will be used as a routine analysis in agricultural products.

Synthesis and Isolation of Monoacetyl-DCB and Diacetyl-DCB from 3,3대-dichlorobenzidine(DCB) (디클로로벤지딘으로부터 대사물질의 합성과 분리방법에 대한 연구)

  • Lee, Jin-Heon;Lee, Beom-Gyu
    • Journal of Environmental Health Sciences
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    • v.29 no.2
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    • pp.50-55
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    • 2003
  • 3,3-dichlorobenzidine is suspected to be cancinogenic in experimental animal and human. Several studies have investigated excretion of metabolites in urine, hemoglobin adduction and cancer incidence among workers occupationally exposed to 3,3'-dichlorobenzidine. In these researches, metabolites of 3,3'-dichlorobenzidine had a very important role, and were required as highly purity. The purpose of this study was synthesis and isolation of its metabolites from 3,3'-dichlorobenzidine. 3,3'-dichlorobenzidine was partially dissolved in benzene, ether, ethanol and methanol, and completely dissolved in 70% acetic acid on mixtures of citric acid containing less than 1% DCB, pyridine, a mixture of 0.5N NaOH and toluene(1:2), and phenol saturated with 20 mM TRIZA base. DCB, monoacetyl-DCB and diacetyl-DCB were measured by using gas chromatography/mass spectrometry(GC/MS). Detection for checking them was nitrogen phosphorous detection mode(NPD), and for identifying them was selected ion monitoring mode(SIM). The base peaks were 252 m/z in DCB, 252, and 294 m/z in monoacetyl-DCB, and 252, 294 and 336 m/z in diacetyl-DCB, respectively. Diacetyl-DCB was synthesized by titrating DCB solution of pyridine with sufficient acetyl chloride. Precipitation was diacetyl-DCB, which was purity of 98.7%. And its supernatant was composed of DCB, monoacetyl-DCB and diacetyl-DCB. By using acetic acid as controller of acetylation, monoacetyl-DCB was isolated from diacetyl-DCB . And residual pyridine was removed by using acetone. The purity of monoacetyl-DCB was 98.8%.

Development of Simultaneous Analysis for the Multi-residual Pesticides in the Ginseng Extract using Gas Chromatography (인삼농축액에서 GC를 이용한 잔류농약 동시다성분 분석법의 개발)

  • Shin Yeong-Min;Lee Seon-Hwa;Son Yeong-Uk;Jeong Ji-Yoon;Jeoung Seoung-Wook;Park Heung-Jai;Kim Sung-Hun;Won Young-Jun;Lee Chang-Hee;Kim Woo-Seong;Hong Moo-Ki;Chae Kab-Ryong
    • Journal of Environmental Science International
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    • v.15 no.1
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    • pp.85-94
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    • 2006
  • The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

Bioequivalence of Nicotine Patches (니코틴 패취제의 생물학적 동등성 평가)

  • 배준호;박은석;지상철
    • Biomolecules & Therapeutics
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    • v.5 no.3
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    • pp.260-264
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    • 1997
  • The bioequivalence of two nicotine patches was evaluated in 16 normal male volunteers (age 21 ~ 27 yrs) following single transdermal application. Test product was "Nicostop patch" made by Sam Yang Co. and reference product was "Nicotinell TTS patch" made by Korean Searle Ciba-Geigy Co. After nicotine patches were applied onto the inside of the forearm, blood was taken at predetermined time intervals and the nicotine concentration in plasma was determined with a sensitive GC method using NPD detector. AUC and Cm\ulcorner were calculated and statistically analyzed for the bioequivalence of the two products. The results showed that the differences in AUC and $C_{msx}$between two products were 5.47% and 2.70%, respectively. The powers (1-$\beta$) for AUC and $C_{max}$. were >90% and 88.76%, respectively. Detectable differences($\Delta$) and confidence intervals were all less than 20%. All of these parameters met the criteria of KFDA for bioequivalence, indicating that "Nicostop patch" is bioequivalent to "Nicotinell TTS patch" . . .

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Lidocaine Intoxication: Two Fatal Cases

  • Lee, Sang-Ki;Lee, Soo-Yeun;In, Sang-Whan;Choi, Hwa-Kyung;Lim, Mi-Ae;Chung, Kyu-Hyuck;Chung, Hee-Sun
    • Archives of Pharmacal Research
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    • v.26 no.4
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    • pp.317-320
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    • 2003
  • We present two fatal cases, a 41-year-old male (case 1) and his 8-year-old daughter (case 2), resulting from acute lidocaine poisoning. Lidocaine was quantified by gas chromatography (GC) analysis using nitrogen-phosphorus detection. The lidocaine concentrations of cases 1 and 2 were: liver, 27.7 $\mu$ g/g and 24.9 $\mu$g/g; spleen, 70.1 $\mu$g/g and 29.9 $\mu$g/g; and gastric contents, 23.6 $\mu$g/g and 42.8 $\mu$g/g, respectively.