• Title/Summary/Keyword: HPLC- MSD

Search Result 44, Processing Time 0.034 seconds

Gas Chromatographic Analysis of TDI, MDI and HDI Using 2-Chlorobenzyl Alcohol and 2,4-Dichlorobenzyl Alcohol Derivatives (2-클로로벤질 알코올 및 2,4-디클로로벤질 알코올 유도체를 이용한 TDI, MDI 및 HDI의 가스크로마토그래피 분석)

  • Yun, Ju-Song;Park, Jun-Ho;Lee, Kang-Myoung;Choi, Hong-Soon;Cho, Young-Bong;Koh, Sang-Baek;Cha, Bong-Suk
    • Journal of Korean Society of Occupational and Environmental Hygiene
    • /
    • v.16 no.3
    • /
    • pp.222-232
    • /
    • 2006
  • Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6-TDI), 4,4'-methylenediphenyl diisocyanate(4,4'-MDI) and 1,6-hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD). Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed. Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were $87^{\circ}C$ and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PD-ECD and GC/MSD. Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.

Simultaneous Analysis of the Coloring Compounds in Indigo, Phellodendron bark, and Madder Dye Using HPLC-DAD-MS

  • Ahn, Cheunsoon;Zeng, Xia;Obendorf, S. Kay
    • Journal of the Korean Society of Clothing and Textiles
    • /
    • v.37 no.6
    • /
    • pp.827-836
    • /
    • 2013
  • Indigotin, indirubin, berberine, palmatine, alizarin, and purpurin are major pigments of indigo plant, Phellodendron bark, and madder. The six pigments were examined using the HPLC-DAD-MS instrument for the purpose of the simultaneous detection of the pigments in a single sample run. The HPLC-DAD-MS method examined the individual pigment solutions in DMSO, a solution containing 6 pigments, and the DMSO extract of the silk dyed with a dye solution of 5 pigments excluding indirubin. The retention times of the HPLC chromatograms, ${\lambda}_{max}$ of the uv-vis absorption bands in the DAD analyses, and the molecular ions detected for the compound peaks in the MSD analyses were consistent throughout the analyses of individual pigment solutions, mixed pigment solutions, and dye extracted from silk dyeing. The developed instrumental method of the simultaneous detection of six pigments can identify dye in an exhumed textile if the textile is dyed using any one (or multiple) pigments of indigo, Phellodendron bark, or madder plant.

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
    • /
    • v.15 no.3
    • /
    • pp.238-245
    • /
    • 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%).

DEVELOPMENT AND COMPARISION OF RESIDUE ANALYSIS FOR BENOMYL IN BEAN AND BEAN SPROUTS (두류와 콩나물에서의 BENOMYL의 검색과 그 분리에 관한 연구)

  • Han, Ilkeun;Chai, Jeungyoung;Lee, Jayoung;Yeo, Ikhyun
    • Analytical Science and Technology
    • /
    • v.7 no.3
    • /
    • pp.395-402
    • /
    • 1994
  • Benomyl(Methyl-1-(Butyl Carbamoyl)-Benzimidazole-2-yl-Carbamate) is widely used as pre- and post-harvest pesticide. It converts into MBC(Carbendarzime:Benzimidazole-2-yl-carbamate) and butyl-isocyanate in mild condition. In this study, three analytical methods for MBC were compared in view of detectability, correctness, and sensitivity. The first and second are HPLC analytical method employing the UV detection of MBC. Our new third method was modification of PFBB(pentafluoro-benzylbromide) derivatization method with GC-ECD & MSD. The average recoveries and detection limit of MBC in the newly modified method are 95% and $0.001{\mu}g/g$ in whole bean and bean sprouts respectively. This new method prevent pesticide analysis from misdetecting in bean and bean sprouts.

  • PDF

Studies on Nutritional Compositions of the Jehotang 2. Organic Acid Content and Volatile Aroma Components (제호탕(醍蝴湯)의 일반영양성분에 관한 연구 2. 유기산 및 휘발성 향기성분 조성)

  • 윤숙자;조후종
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.25 no.4
    • /
    • pp.654-658
    • /
    • 1996
  • Organic acid content and volatile aroma components in Jehotang were investigated. Organic acids were detceted by HPLC and it is composed of formic acid(0.07%). lactic acid(0.22%) acetic acid (0.32%), and citric acid(3.17%), the last of which is one of the noteworthy features of Jehotang contributing greatly to its sour flavor and taste. Among the 39 volatile aroma components, whose peaks were identified by GC/MSD, and whose structures were analyzable, 17 kinds of hydrocarbon(30.81%) one kind of aldehyde(7.18%), 2 kinds of ketone(4.79%), 8 kinds of terpene(25.96%) a variety of acids (16%), 2 kinds of alcohol(5.42%), 2 kinds of phenol(2.76%) and 3 kinds of the others(7.68%) were found. The hydrocarbons, terpenes and acids occupied 70% of the aroma components, contributing to and also composing the particular flavor of Jehotang. Extracted pigments from the Jehotang showed maximum light absorbance in the wave length ranges of 200~400nm, showing a high degree of light adsorption of yellow to red color.

  • PDF

Monitoring of pesticide residues in commercial agricultural products in the northern area of Seoul, Korea (서울 북부지역 유통 농산물의 농약 잔류실태)

  • Han, Sung-Hee;Park, Sung-Kyu;Kim, Ouk-Hee;Choi, Young-Hee;Seoung, Hyun-Jung;Lee, Young-Ju;Jung, Jung-Hee;Kim, Yun-Hee;Yu, In-Sil;Kim, Yoo-Kyung;Han, Ki-Young;Chae, Young-Zoo
    • The Korean Journal of Pesticide Science
    • /
    • v.16 no.2
    • /
    • pp.109-120
    • /
    • 2012
  • This study was conducted to monitor 284 pesticides residue level in 2,914 commercial agricultural products in the northern area of Seoul in 2011 by the multi class pesticide multiresidue analysis methods in Korea Food Code using GC, HPLC, GC-MSD and, LC-MSD. The detection rate of pesticide residues were 14.8% (431/2,914). The order of agricultural products in which the pesticide residues were detected was perilla leaves 40.0% (28/70), chamnamul 35.5% (11/31), amaranth 30.0% (3/10) and spinach 27.7% (38/137) etc. The percentage of products that exceeded the MRLs (maximum residue limits) were 1.0% (31/431). Those products that exceeded MRLs were ginseng (6), perilla leaves (4), leek (4), welsh onion (3) and sedeum (3) etc. The 59 kinds of the pesticides were detected on this study, 21 pesticides of them were detected over MRLs. Detection rate of fungicides (56.4%) was higher than that of insecticides (42.1%). And procymidone was detected with considerable high frequency. Additionally, residual residual violates pesticides were in the order of tolclofos-methyl, endosulfan, dimethomorph, diniconazole and fludioxonil. According to the agricultural marketing channels, detection and excess rate of them were monitored. Detection and excess rate of samples circulated in agricultural traditional market were highest. The estimated daily intakes (EDI) of the pesticides were compared to personal acceptable daily intakes (PADI) in order to risk assessment by food consumption. Diazinon in Korean cabbage showed the highest %ADI, 2.9901 and others showed below 3.0 %ADI. Overall, these results indicate that residue levels of pesticides detected were evaluated as safe.

Monitoring and Risk Assessment of Pesticide Residues in Commercial Environment Friendly Fruits and Fruiting Vegetables (유통 친환경 과실류와 과채류 중 농약잔류 실태조사 및 안전성 평가)

  • Lee, Jae Yun;Noh, Hyun Ho;Park, So Hyun;Lee, Kwang Hun;Park, Hyo Kyoung;Hong, Su Myeong;Kim, Doo Ho;Kyung, Kee Sung
    • The Korean Journal of Pesticide Science
    • /
    • v.16 no.4
    • /
    • pp.308-314
    • /
    • 2012
  • In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

Monitoring and Risk Assessment of Pesticide Residues in Agricultural Products Collected from Wholesale and Traditional Markets in Cheongju (청주지역 유통 농산물 중 잔류농약 모니터링 및 안전성 평가)

  • Noh, Hyun-Ho;Kang, Kyung-Won;Park, Young-Soon;Park, Hyo-Kyung;Lee, Kwang-Hun;Lee, Jae-Yun;Yeop, Kyung-Won;Lee, Eun-Young;Jin, Yong-Duk;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
    • /
    • v.14 no.1
    • /
    • pp.1-9
    • /
    • 2010
  • In order to survey residual characteristics of pesticides in the agricultural products selling at markets and to assess their safety, a total of 120 agricultural products were collected from the wholesale and traditional markets in Cheongju and analyzed the pesticide residues in them by multiresidue analysis method using GLC, HPLC and GC-MSD. Three pesticides, procymidone, penconazole, and tetraconazole, were detected from 4 samples such as onion, leek, tomato, and green pepper. Fungicide penconazole was detected from the onion collected from wholesale market. Fungicide procymidone was detected from leek and tomato and fungicide tetraconazole was detected from green pepper. Pesticide residues were detected from 3.3% of the total samples. The estimated daily intakes (EDIs) of the pesticides detected were less than 0.1% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe.

Characteristics of Thiosulfinates and Volatile Sulfur Compounds from Blanched Garlic Reacted with Alliinase (Alliinase 첨가에 의한 열처리 마늘로부터 생성된 함황 화합물의 특성)

  • Choi, Yoon-Hee;Shim, You-Sin;Kim, Cheong-Tae;Lee, Chan;Shin, Dong-Bin
    • Korean Journal of Food Science and Technology
    • /
    • v.39 no.6
    • /
    • pp.600-607
    • /
    • 2007
  • In this study, attempts were made to develop a method for controlling the volatile sulfur compounds in garlic. Crude alliinase extracted from fresh garlic was applied to garlic pulp blanched far 5 min at $100^{\circ}C$, and the changes in the thiosulfinates and volatile compounds of the blanched garlic pulp reacted with the enzyme were investigated. Eight kinds of thiosulfinates from garlic were separated by HPLC, and identified by LC/MS/MS. When the alliinase was added to the blanched garlic pulp at 100, 200, 300, or 400 units, and reacted for 15 min, respectively, thiosulfinates were generated in the amounts of 37, 68, 77, and 80% of the fresh garlic content (control). Under the same conditions, we analyzed the volatile compounds, where 28 peaks were identified by GC/MSD. Of the 28 peaks, 23 were volatile sulfur compounds. The results of the analysis showed that all the volatile compounds were generated at amounts of 25, 36, 66, and 76% of the content of the control, respectively. These results indicate that the sulfur compound content of garlic can be regulated, depending upon the reaction conditions of allinase.

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
    • /
    • v.21 no.1
    • /
    • pp.69-74
    • /
    • 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.