• Title/Summary/Keyword: GC-MS (gas chromatographic-mass spectrometry)

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High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Quality Evaluation of the Cinnamon Essential Oils Based on Gas Chromatographic Analysis and Cytotoxicity (가스 크로마토그래피 분석과 세포독성에 의한 계피 정유의 품질평가)

  • Jung, Hyun-Ju;Jung, Won-Tae;Choi, Jong-Won;Nam, Jung-Hwan;Lee, Kyung-Tae;Kwon, Byung-Mok;Park, Hee-Juhn
    • Korean Journal of Pharmacognosy
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    • v.35 no.4 s.139
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    • pp.288-292
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    • 2004
  • To evaluate the quality of the crude drugs using three kinds of Cinnamomum Cortex (CC), Vietnamese CC (VCC, the stem bark of Cinnamomum obtusifolium), periderm-peeled Chinese CC (PPCC, periderm-peeled stem bark of C. cassia), Chinese CC (CCC, stem bark of C. cassia) and a Cinnamomi Ramulus (CR, the twig of C. cassia), the four essential oils were prepared by steam distillation method. Cinnamaldehdye (CAN) and an unknown substance tentatively named hydroxy-cinnamaldehdye(HCNA) were detected in the four essential oils by gas chromatography-mass spectrometry, the contents of which are significantly different one another. Vietnamese CC had the highest content of HCNA whereas CR had the highest CAN content and the lowest HCNA. Vietnamese CC exhibited the greatest cytotoxic activity against the cancer cell lines, A549, HepG-2, HL-60, P-388, U-937, and KB and CR the lowest cytotoxicity. Contents of CAN and HCNA in CCC and PPCC are positioned between VCC and CR. These results suggest that measurement of HCNA and cytotoxicity may determine the quality of CC and CR.

Performance Evaluation of Hazardous Substances using Measurement Vehicle of Field Mode through Emergency Response of Chemical Incidents

  • Lee, Yeon-Hee;Hwang, Seung-Ryul;Kim, Jae-Young;Kim, Kyun;Kwak, Ji Hyun;Kim, Min Sun;Park, Joong Don;Jeon, Junho;Kim, Ki Joon;Lee, Jin Hwan
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.294-302
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    • 2015
  • BACKGROUND: Chemical accidents have increased owing to chemical usage, human error and technical failures during the last decades. Many countries have organized supervisory authorities in charge of enforcing related rules and regulations to prevent chemical accidents. A very important part in chemical accidents has been coping with comprehensive first aid tool. Therefore, the present research has provided information with the initial applications concern to the rapid analysis of hazardous material using instruments in vehicle of field mode after chemical accidents. METHODS AND RESULTS: Mobile measurement vehicle was manufactured to obtain information regarding field assessments of chemical accidents. This vehicle was equipped with four instruments including gas chromatography with mass spectrometry (GC/MS), Fourier Transform Infrared Spectroscopy (FT-IR), Ion Chromatography (IC), and UV/Vis spectrometer (UV) to analyses of accident preparedness substances, volatile compounds, and organic gases. Moreover, this work was the first examined the evaluation of applicability for analysis instruments using 20 chemicals in various accident preparedness substances (GC/MS; 6 chemicals, FT-IR; 2 chemicals, IC; 11 chemicals, and UV; 1 chemical) and their calibration curves were obtained with high linearity ( r 2 > 0.991). Our results were observed the advantage of the high chromatographic peak capacity, fast analysis, and good sensitivity as well as resolution. CONCLUSION: When chemical accidents are occurred, the posted measurement vehicle may be utilized as tool an effective for qualitative and quantitative information in the scene of an accident owing to the rapid analysis of hazardous material.

Phytochemical Analysis and Anti-cancer Investigation of Boswellia Serrata Bioactive Constituents In Vitro

  • Ahmed, Hanaa H;Abd-Rabou, Ahmed A;Hassan, Amal Z;Kotob, Soheir E
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7179-7188
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    • 2015
  • Cancer is a major health obstacle around the world, with hepatocellular carcinoma (HCC) and colorectal cancer (CRC) as major causes of morbidity and mortality. Nowadays, there isgrowing interest in the therapeutic use of natural products for HCC and CRC, owing to the anticancer activity of their bioactive constituents. Boswellia serrata oleo gum resin has long been used in Ayurvedic and traditional Chinese medicine to alleviate a variety of health problems such as inflammatory and arthritic diseases. The current study aimed to identify and explore the in vitro anticancer effect of B. Serrata bioactive constituents on HepG2 and HCT 116 cell lines. Phytochemical analysis of volatile oils of B. Serrata oleo gum resin was carried out using gas chromatography-mass spectrometry (GC/MS). Oleo-gum-resin of B. Serrata was then successively extracted with petroleum ether (extract 1) and methanol (extract 2). Gas-liquid chromatography (GLC) analysis of the lipoidal matter was also performed. In addition, a methanol extract of B. Serrata oleo gum resin was phytochemically studied using column chromatography (CC) and thin layer chromatography (TLC) to obtain four fractions (I, II, III and IV). Sephadex columns were used to isolate ${\beta}$-boswellic acid and identification of the pure compound was done using UV, mass spectra, $^1H$ NMR and $^{13}C$ NMR analysis. Total extracts, fractions and volatile oils of B. Serrata oleo-gum resin were subsequently applied to HCC cells (HepG2 cell line) and CRC cells (HCT 116 cell line) to assess their cytotoxic effects. GLC analysis of the lipoidal matter resulted in identification of tricosane (75.32%) as a major compound with the presence of cholesterol, stigmasterol and ${\beta}$-sitosterol. Twenty two fatty acids were identified of which saturated fatty acids represented 25.6% and unsaturated fatty acids 74.4% of the total saponifiable fraction. GC/MS analysis of three chromatographic fractions (I,II and III) of B. Serrata oleo gum resin revealed the presence of pent-2-ene-1,4-dione, 2-methyl- levulinic acid methyl ester, 3,5- dimethyl- 1-hexane, methyl-1-methylpentadecanoate, 1,1- dimethoxy cyclohexane, 1-methoxy-4-(1-propenyl)benzene and 17a-hydroxy-17a-cyano, preg-4-en-3-one. GC/MS analysis of volatile oils of B. Serrata oleo gum resin revealed the presence of sabinene (19.11%), terpinen-4-ol (14.64%) and terpinyl acetate (13.01%) as major constituents. The anti-cancer effect of two extracts (1 and 2) and four fractions (I, II, III and IV) as well as volatile oils of B. Serrata oleo gum resin on HepG2 and HCT 116 cell lines was investigated using SRB assay. Regarding HepG2 cell line, extracts 1 and 2 elicited the most pronounced cytotoxic activity with $IC_{50}$ values equal 1.58 and $5.82{\mu}g/mL$ at 48 h, respectively which were comparable to doxorubicin with an $IC_{50}$ equal $4.68{\mu}g/mL$ at 48 h. With respect to HCT 116 cells, extracts 1 and 2 exhibited the most obvious cytotoxic effect; with $IC_{50}$ values equal 0.12 and $6.59{\mu}g/mL$ at 48 h, respectively which were comparable to 5-fluorouracil with an $IC_{50}$ equal $3.43{\mu}g/mL$ at 48 h. In conclusion, total extracts, fractions and volatile oils of B. Serrata oleo gum resin proved their usefulness as cytotoxic mediators against HepG2 and HCT 116 cell lines with different potentiality (extracts > fractions > volatile oil). In the two studied cell lines the cytotoxic acivity of each of extract 1 and 2 was comparable to doxorubicin and 5-fluorouracil, respectively. Extensive in vivo research is warranted to explore the precise molecular mechanisms of these bioactive natural products in cytotoxicity against HCC and CRC cells.