scholarly journals Quantification of acrylamide in foods selected by using gas chromatography tandem mass spectrometry

2016 ◽  
Vol 70 (2) ◽  
pp. 209-215 ◽  
Author(s):  
Veselin Delevic ◽  
Refik Zejnilovic ◽  
Biljana Jancic-Stojanovic ◽  
Brizita Djordjevic ◽  
Zorana Tokic ◽  
...  
Keyword(s):  
Solid Phase ◽  
Water Solution ◽  
Sodium Thiosulfate ◽  
Water Extract ◽  
Coefficient Of Determination ◽  
Bromine Water ◽  
Reduced Volume ◽  
Sample Homogenization ◽  
Carcinogenic Compound

Acrylamide is toxic and probably carcinogenic compound, made as a result of high-temperature thermal treatment of carbohydrate-rich foodstuffs. In this article a method is improved for the extraction and quantitation of acrylamide in foods produced based on corn flour that are represented in our traditional diet. Acrylamide extraction was carried out using reduced volume of saturated solution of bromine water and the GC - MS method for the quantification was shown. Quantification of acrylamide was preceded by: sample homogenization, acrylamide extraction using water, extract purification using solid phase extraction, bromination, using a reduced volume of bromine water solution, dehydrobromination with sodium thiosulfate and transformation of dibromopropenamide in 2,3- 2- bromopropenamide using triethylamine. Regression and correlation analysis were applied for the probability level of 0.05. Calibration is performed in the concentration range 5-80 ug/kg with a detection limit 6.86 mg / kg and the limits of quantification 10.78 ug/kg and the coefficient of determination R2 > 0.999. Calibration curve was obtained: y = 0,069x + 0,038. Recovery values were an average from 97 to 110%. Proposed GC-MS method is simple, precise and reliable for the determination of acrylamide in the samples of thermal treated foods. Our results show that the tested foods quantify the presence of acrylamide in concentrations of 18 to 77 mg/kg acrylamide depending on whether the food was prepared by cooking or baking.

scholarly journals Multiresidue Analytical Method for the Determination of Eight Penicillin Antibiotics in Muscle Tissue by Ion-Pair Reversed-Phase HPLC after Precolumn Derivatization

1999 ◽  
Vol 82 (5) ◽  
pp. 1083-1095 ◽  
Author(s):  
Eric Verdon ◽  
Pierrick Couëdor
Keyword(s):  
Muscle Tissue ◽  
Phosphate Buffer ◽  
High Performance ◽  
Solid Phase ◽  
Sodium Thiosulfate ◽  
Reversed Phase ◽  
Extraction Column ◽  
Precolumn Derivatization ◽  
Solution Ph

Abstract A high-performance liquid chromatographic multiresidue method was developed for the determination of 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer pH 9 followed by cleanup and concentration on a C18 solid¯phase extraction column and reaction with benzoic anhydride at 50°C for 5 min and with 1,2,4-triazole and mercury(II) chloride solution pH 9 at 65°C for 10 min. The derivatized compounds are eluted on a C18 column with a mobile phase containing acetonitrile and phosphate buffer (pH 6; 0.1 mol/L) loaded with sodium thiosulfate and ion-pairing tetrabutylammonium hydrogenosulphate. The method detection limit is approximately 3-11 μg/kg and the limit of determination was evaluated down to 25 μg/kg in line with the criteria of the EU decision No. 93/256/EEC.

The Determination of Galaxolide in Water Samples with SPME Coupled with GC-MS

2011 ◽  
Vol 183-185 ◽  
pp. 184-187
Author(s):  
Bi Dong Su ◽  
Chen Zhen Min ◽  
Chen Dong Hui
Keyword(s):  
River Water ◽  
Solid Phase Microextraction ◽  
Extraction Efficiency ◽  
Solid Phase ◽  
Water Solution ◽  
Mass Spectrometric ◽  
Limit Of Quantification ◽  
Urban Sewage ◽  
Direct Sampling

Described is a solid-phase microextraction-gas chromatography mass spectrometric procedure for the determination of galaxolide (HHCB) in water solution samples. In which 100 μm PDMS coated fiber were used. From the optimization experiments of SPME, we found the direct sampling is necessary. The extraction time and temperature were 40min and 35°C, respectively. the salinity of the solution almost has no effect on the extraction efficiency and pH=7.0 was suitable for the extraction of HHCB. The method were applied to the urban sewage and river water respectively and found the content of HHCB in the urban sewage is 286ng/L, while those in river water below limit of quantification.

scholarly journals Chromatographic Analysis (LC-MS and GC-MS), Antioxidant Activity, Total Phenol and Total Flavonoid Determination of Ononis natrix L. Grown in Jordan

2021 ◽  
Vol 16 (1) ◽  
pp. 31-39
Keyword(s):  
Solid Phase ◽  
Water Extract ◽  
Ethanol Extract ◽  
Total Phenol ◽  
Aroma Profile ◽  
Sesquiterpene Hydrocarbons ◽  
Leaf Oil ◽  
Terpenoid Aldehydes ◽  
Ethanol Extracts

The purpose of the present study was to identify, by gas chromatography (GC) and GC-mass spectrometry (GC-MS), the components of the spontaneously emitted volatile organic compounds (VOCs), obtained by Solid-Phase-Micro-Extraction (SPME) and that of the hydrodistilled oil of the fresh flowers and leaves of Ononis natrix, as well as to compare them. The hydrodistilled leaf oil was rich in non-terpenoid aldehydes, whereas its aroma profile contained mainly sesquiterpene hydrocarbons with α-copaene and germacrene D as their major components. The hydrodistilled oil of the fresh flowers, however, revealed nearly equal amounts of terpenoid and non-terpenoid compounds; 51.00% and 46.54%, respectively. The aroma profile of the fresh flowers was dominated by monoterpene hydrocarbons with α-pinene (42.96%) and α-thujene (20.17%) as the predomi¬nant two monoterpenes. Based on the high total phenol and flavonoid contents of the water and ethanol extracts, LC-MS analysis was carried out to identify the major compounds from each sample. From the water extract, eleven compounds were identified, whereas the ethanol extract contained eight, whereby luteolin (from the water extract) and apigenin (from the ethanol one) were named as the major flavonoids, respectively.

scholarly journals Simultaneous determination of fluoride and monofluorophosphate in toothpastes by supressed ion chromatography

2006 ◽  
Vol 4 (4) ◽  
pp. 798-807 ◽  
Author(s):  
Rajmund Michalski ◽  
Barbara Mathews
Keyword(s):  
Ion Chromatography ◽  
Solid Phase ◽  
High Capacity ◽  
Coefficient Of Determination ◽  
Anion Exchange Column ◽  
Total Uncertainty ◽  
Minimal Sample ◽  
Solid Phase Extraction Cartridge ◽  
Total Analysis

AbstractSuppressed ion chromatography with a highly selective and high capacity anion-exchange column is used for the determination of anionic compounds in ten commercially available toothpastes. Minimal sample preparation is needed, requiring only dilution and filtration over a solid-phase extraction cartridge. Quantitative analysis of fluoride and monofluorophosphate, as well as chloride, nitrate, orthophosphate, and sulfate is achieved in one chromatographic run with a total analysis time of 25 minutes.Optimized analytical conditions are validated in terms of accuracy, precision, and total uncertainty, and the results demonstrate the reproducibility of ion chromatography. The coefficient of determination for the anions ranges from 0.9896 to 0.9997. The spiked recoveries for the anions are 88–108%. The change in the fluoride content of the toothpaste with storage time is investigated.

Determination of Pesticide in Soil-Water System by Solid Phase Extraction and Gas Chromatography

2013 ◽  
Vol 781-784 ◽  
pp. 2221-2224
Author(s):  
Hong Bin Wang ◽  
Mei Bai ◽  
Wei Tan ◽  
Yun Tao Gao ◽  
Yong Jun Yang ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Soil Water ◽  
Solid Phase ◽  
Water Solution ◽  
Water System ◽  
Phase Extraction ◽  
Standard Curve ◽  
Relative Standard

A SPE-GC-FID method was developed for the analyzing the residues of prometryne and acetochlor in soil-water system. The sample solution was made up of the standard stock solution of prometryne-acetochlor and soil-water solution with a certain proportion.purified by C18solid-phase extraction (SPE) column, and then leached by acetone. The leached was filtrated with microporous membrane (d<0.45 μm). The results showed that the standard curve was showed in the range of 1.5~30 μg/mL with a correlation coefficient of 0.9995 and 0.9980. The recoveries (n=5) were 98.9%~107.2%, with relative standard deviation ranged from 2.52% to 9.7%.The detection limits of prometryne was 0.22 μg/mL and acetochlor was 0.19 μg/mL. This method provides a dependable approach to examine and evaluate the residues of prometryne and acetochlor in the soil-water system.

scholarly journals Determination of Mepiquat Chloride Residues in Cotton and Soil by Liquid Chromatography/Mass Spectrometry

2008 ◽  
Vol 91 (5) ◽  
pp. 1110-1115 ◽  
Author(s):  
Xin-Gang Liu ◽  
Feng-Shou Dong ◽  
Shuo Li ◽  
Yong-Quan Zheng
Keyword(s):  
Solid Phase ◽  
Calibration Graph ◽  
Coefficient Of Determination ◽  
Mepiquat Chloride ◽  
Relative Standard ◽  
Cotton Seeds ◽  
Liquid Chromatographic ◽  
Positive Ion ◽  
Chromatographic Mass

Abstract A liquid chromatographic/mass spectrometric (LC/MS) method is reported for the determination of the onium-type plant growth regulator mepiquat chloride in cotton and soil. The pesticide was extracted from the sample with ethanol and water containing 2 NH4Cl. The extract was cleaned up on a solid-phase extraction C18 column, and the pesticide was determined by LC/MS. The average recoveries were 85.993.8, 81.391.7, and 78.194.7, with corresponding relative standard deviations of 3.49.6, 3.712.3, and 4.09.8, from soil, cotton leaves, and cotton seeds, respectively. A coefficient of determination of R2 0.9964 was obtained for the analyte calibration graph, from 0.05 to 100 g/mL. Decision limits, CC, and detection capability, CC, were calculated. Electrospray ionization LC/MS in the positive-ion mode (ESI+) was used to detect mepiquat chloride in extracts of soil, cotton leaves, and cotton seeds. The ion at m/z 114 in the mass spectrum was monitored.

Modern determinants of endometrium hyperplastic processes pathogenesis

2016 ◽  
pp. 137-142
Author(s):  
V.O. Benyuk ◽  
◽  
V.M. Goncharenko ◽  
T.R. Nykoniuk ◽  
◽  
...  
Keyword(s):  
Conservative Therapy ◽  
Solid Phase ◽  
Research Direction ◽  
Immunohistochemical Method ◽  
Results Of Treatment ◽  
Treatment And Prevention ◽  
Receptor Phenotype ◽  
The Relationship ◽  
Endometrial Proliferation

The objective: to еxplore the relationship between the activity of endometrial proliferation and the state of the local immune response in the uterus in the conditions berprestasi process. Patients and methods. Examined 228 women of reproductive and perimenopausal age with endometrial pathology using ultrasound and then performing hysteroresectoscopy. Determination of the concentrations of the cytokines IL-1, IL-2, IL-6 and TNF was performed by solid phase ELISA. Results. Found a trend that confirms the loss of sensitivity to hormones at the stage of malignancy of the endometrium and can be used as diagnostic determinants in determining the nature of intrauterine pathology and criterion of the effectiveness of conservative therapy. Conclusion. Improving etiopatogenetice approach to the therapy of hyperplastic proce.sses of endometrium with determination of receptor phenotype of the endometrium is a research direction in modern gynecology, which will help to improve the results of treatment and prevention of intrauterine pathology. Key words: endometrial hyperplasia,the receptors for progesterone and estrogen, immunohistochemical method.

Laboratory Determination of the Solid Phase Composition of Technogenically Salinized Peatlands: Possibilities and Limitations

2020 ◽  
Vol 75 (3) ◽  
pp. 131-137
Author(s):  
Yu. N. Vodyanitskii ◽  
N. A. Avetov ◽  
A. T. Savichev ◽  
S. Ya. Trofimov ◽  
E. A. Shishkonakova
Keyword(s):  
Phase Composition ◽  
Solid Phase ◽  
Laboratory Determination ◽  
Solid Phase Composition
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