Evaluation and validation of two different chromatographic methods (HPLC and LC-MS/MS) for the determination and confirmation of ochratoxin A in pig tissues

This study was undertaken to compare two different analytical methods for the determination and confirmation of ochratoxin A (OTA) in blood serum, kidney and liver of pigs. Sample clean-up was based on liquid-liquid phase extraction. The detection of OTA was accomplished with high-performance liquid chromatography (HPLC) combined either with fluorescence detection (FL) or electro spray ionization (ESI+) tandem mass spectrometry (MS–MS). Comparative method evaluation was based on the investigation of 90 samples of blood serum, kidney and liver per animal originating from different regions of Serbia. The analytical results are discussed in view of the respective method validation data and the corresponding experimental protocols. In general, analytical data obtained with (LC–MS–MS) liquid chromatography electro spray tandem mass spectro metry detection offered comparable good results at the sub-ppb concentration level. The results indicate that the liquid chromatography electro spray tandem mass spectrometric (LC-MS/MS) method was more specific and sensitive for the analysis and confirmation of ochratoxin A in pig tissues then high pressure liquid chromatography (HPLC) method after methylation of OTA.     

Method development,validation, monitoring,seasonal effect and risk assessment of multiclass multi pesticide residues in surface and ground water of new alluvial zone in eastern India

Environmental Science and Pollution Research - A liquid–liquid extraction (LLE) method was validated as per SANTE/12682/2019 guidelines for gas chromatography–mass spectrometric...     

Gas chromatographic and mass spectrometric characterization of terbufos sulfoxide and its hydration product

Abstract

Terbufos sulfoxide is a primary metabolite of the organophosphorus insecticide terbufos. The identification of terbufos sulfoxide was determined by combined gas chromatography/mass spectrometry and the direct probe. Mass spectral data are presented and discussed. The data indicate that thermal degradation occurred in the heated GC column. A hydration product of terbufos sulfoxide was detected and its mass spectral data are discussed.     

焦化厂A/O出水中的有机污染物分析

采用色谱－质谱（GC／MS）联用仪分析和鉴定了上海宝钢焦化厂A／O生化阶段出水的有机污染物组成,共检出各类有机污染物70多种。结合焦化废水专用混凝剂的混凝处理实验结果,指出了各类有机污染物的去除情况。     

Application of automated mass spectrometry deconvolution and identification software for pesticide analysis in surface waters

A new approach to surface water analysis has been investigated in order to enhance the detection of different organic contaminants in Nathan Creek, British Columbia. Water samples from Nathan Creek were prepared by liquid/liquid extraction using dichloromethane (DCM) as an extraction solvent and analyzed by gas chromatography mass spectrometry method in scan mode (GC-MS scan). To increase sensitivity for pesticides detection, acquired scan data were further analyzed by Automated Mass Spectrometry Deconvolution and Identification Software (AMDIS) incorporated into the Agilent Deconvolution Reporting Software (DRS), which also includes mass spectral libraries for 567 pesticides. Extracts were reanalyzed by gas chromatography mass spectrometry single ion monitoring (GC-MS-SIM) to confirm and quantitate detected pesticides. Pesticides: atrazine, dimethoate, diazinone, metalaxyl, myclobutanil, napropamide, oxadiazon, propazine and simazine were detected at three sampling sites on the mainstream of the Nathan Creek. Results of the study are further discussed in terms of detectivity and identification level for each pesticide found. The proposed approach of monitoring pesticides in surface waters enables their detection and identification at trace levels.     

Evaluation of the treatment efficiencies of paper mill whitewaters in terms of organic composition and toxicity

The efficiency of several lab scale treatments (aerobic, anaerobic and ozone or combination of these) was evaluated using two packaging board mill whitewaters. The effect of the different treatments on the elimination of the organic load, the chemical oxygen demand (COD) and the toxicity was tested as well as the relationship between these parameters. Biocides, phenolic compounds, surfactants, plasticiziers and wood extractives were identified in untreated and treated whitewaters by liquid chromatography coupled with mass spectrometry (LC-MS) or gas chromatography coupled with mass spectrometry (GC-MS). A strong dependency on the water type and treatment efficiency was observed, being the combination of anaerobic and aerobic treatments the best option to reduce the organic contaminants in these waters, although in some cases, the toxicity did not decrease. However, ozone as post-treatment permitted a further reduction of organic compounds, toxicity and COD.     

Analysis of target and nontarget pollutants in aqueous leachates from the hazardous waste site Stringfellow, California, via ion chromatography - particle beam and inductively coupled plasma mass spectrometry

Liquid chromatography particle beam mass spectrometry (PB/MS is a powerful tool for the analysis of target pollutants but complementary methods are required for nontarget compounds. Preliminary data are presented on an anion exchange chromatography PB/MS based method for the detection of the target compound 4-chlorobenzene sulfonic acid (a contamlnant found in hazardous waste leachates) and also for nontarget pollutants in aqueous leachate samples from the Stringfellow hazardous waste site in California. Anion exchange chromatography coupled to inductively coupled plasma mass spectrometry yields qualitative and quantltative elemental analysis showing the presence or absence of key heteroatoms in organic pollutants including chlorine, other halogens, phosphorus and sulfur.     

A study into the parameters affecting selected reaction monitoring of 2,3,7,8-TCDD

The use of high resolution (10,000 resolving power) coupled gas chromatography - mass spectrometry is a well established technique in the analysis of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) but in the case of heavily contaminated stack samples interferences can still occur. A complementary technique that offers high specificity is selected reaction monitoring (SRM).A study has been made into the effects that affect the metastable dissociation of 2,3,7,8-TCDD in the first field free region (FFR1) of a magnetic sector mass spectrometer, and monitored using SRM.Monatomic, diatomic and polyatomic gases have been investigated in the collision chamber of the mass spectrometer, as have the effects of electron energy, source temperature and trap current on the dissociation, and optima conditions determined for them.     

Application of Automated Mass Spectrometry Deconvolution and Identification Software for Pesticide Analysis in Surface Waters

A new approach to surface water analysis has been investigated in order to enhance the detection of different organic contaminants in Nathan Creek, British Columbia. Water samples from Nathan Creek were prepared by liquid/liquid extraction using dichloromethane (DCM) as an extraction solvent and analyzed by gas chromatography mass spectrometry method in scan mode (GC-MS scan). To increase sensitivity for pesticides detection, acquired scan data were further analyzed by Automated Mass Spectrometry Deconvolution and Identification Software (AMDIS) incorporated into the Agilent Deconvolution Reporting Software (DRS), which also includes mass spectral libraries for 567 pesticides. Extracts were reanalyzed by gas chromatography mass spectrometry single ion monitoring (GC-MS-SIM) to confirm and quantitate detected pesticides. Pesticides: atrazine, dimethoate, diazinone, metalaxyl, myclobutanil, napropamide, oxadiazon, propazine and simazine were detected at three sampling sites on the mainstream of the Nathan Creek. Results of the study are further discussed in terms of detectivity and identification level for each pesticide found. The proposed approach of monitoring pesticides in surface waters enables their detection and identification at trace levels.     

离子色谱在饮用水消毒副产物及高氯酸盐分析中的应用

介绍了离子色谱在饮用水中消毒副产物及高氯酸盐分析中的应用。重点介绍了离子色谱测定饮用水中溴酸盐和高氯酸盐的方法。简单介绍了卤代乙酸和氯酸盐的离子色谱测定法及离子色谱-质谱联用技术在饮用水消毒副产物及高氯酸盐分析中的应用。     

Sampling and Analysis of Volatile Organic Compounds Evolved During Thermal Processing of Acrylonitrile Butadiene Styrene Composite Resins

Abstract

The evaluation of emissions of volatile organic compounds (VOCs) during processing of resins is of interest to resin manufacturers and resin processors. An accurate estimate of the VOCs emitted from resin processing has been difficult due to the wide variation in processing facilities. This study was designed to estimate the emissions in terms of mass of emitted VOC per mass of resin processed.

A collection and analysis method was developed and validated for the determination of VOCs present in the emissions of thermally processed acrylonitrile butadiene styrene (ABS) resins. Four composite resins were blended from automotive, general molding, pipe, and refrigeration grade ABS resins obtained from the manufacturers. Emission samples were collected in evacuated 6-L Summa canisters and then analyzed using gas chromatography/flame ionization detection/mass selective detection (GC/FID/MSD). Levels were determined for nine target analytes detected in canister samples, and for total VOCs detected by an inline GC/FID. The emissions evolved from the extrusion of each composite resin were expressed in terms of mass of VOCs per mass of processed resin. Styrene was the principal volatile emission from all the composite resins. VOCs analyzed from the pipe resin sample contained the highest level of styrene at 402 μg/g. An additional collection and detection method was used to determine the presence of aerosols in the emissions. This method involved collecting particulates on glass fiber filters, extracting them with solvents, and analyzing them using gas chromatography/mass spectrometry (GC/MS). No significant levels of any of the target analytes were detected on the filters.     

New Evidence for the presence of arsenocholine in shrimps (Pandalus borealis) by use of pyrolysis gas chromatography — atomic absorption spectrometry/mass spectrometry

An analytical method for the structure elucidation of quarternary organoarsenic compounds in trace amounts in fish and crustaceans has been developed in this laboratory. The two major organoarsenicals found in shrimps have been separated by ion-exchange chromatography and their stucture has been studied by the use of pyrolysis gas chromatography. Their degradation in the pyrolyzer unit has been studied by the use of atomic absorption spectrophotometer or mass spectrometer as detectors. A comparison of the analytical data of these substances and data from synthetic reference substances show complete agreement. The structures of reference compounds have been confirmed by use of nuclear magnetic resonance spectrometry and fast atom bombardment (FAB) mass spectrometry. It is demonstrated that both of the organoarsenic compounds in shrimps have a trimethylarsonio moiety e.g. the compounds have a quarternary structure. Furthermore, the more basic organoarsenic compound has a mass spectrometric fragmentation pattern similar to synthetic arsenocholine and acetylarsenocholine. Treatment of arsenobetaine with hot base produces trimethylarsineoxide in a high yield (96%). Arsenocholine, however, remains unchanged during this treatment. Treatment with sodium benzenethiolate does not result in chemical demethylation, which shows that this method together with gas chromatography-mass spectrometry is not feasible for confirmation of its structure.     

Multiresidue analysis of pesticides in fruits and vegetables by gas chromatography-mass spectrometry

A multiresidue method was assessed for the determination of several pesticides (organochlorine, organophosphorus, pyrethroids, triazole, amidine) using gas chromatography/mass spectrometry. The extraction of pesticides was carried out by liquid-liquid extraction (LLE) and solid-phase extraction (SPE) using two types of columns (CN and C18). The extracts were cleaned by the addition of florisil, the pesticides were separated by capillary column gas chromatography and detected by mass spectrometry in the electron impact mode. The extraction using C18 column provided the best results for most of the analyzed pesticides. The majority of pesticides recoveries from the four fruits and vegetables (apples, pears, tomatoes and pepper) were greater than 60%. Linearity and precision were satisfactory. The estimated limits of detection and limits of quantification ranged from 0.01 to 0.1 mg/kg and from 0.02 to 0.3 mg/kg, respectively. The proposed procedure was found to be useful for the multiresidue analyses of pesticides in agricultural products for routine monitoring programs.     

Multiresidue analysis of pesticides in fruits and vegetables by gas chromatography-mass spectrometry

A multiresidue method was assessed for the determination of several pesticides (organochlorine, organophosphorus, pyrethroids, triazole, amidine) using gas chromatography/mass spectrometry. The extraction of pesticides was carried out by liquid-liquid extraction (LLE) and solid-phase extraction (SPE) using two types of columns (CN and C18). The extracts were cleaned by the addition of florisil, the pesticides were separated by capillary column gas chromatography and detected by mass spectrometry in the electron impact mode. The extraction using C18 column provided the best results for most of the analyzed pesticides. The majority of pesticides recoveries from the four fruits and vegetables (apples, pears, tomatoes and pepper) were greater than 60%. Linearity and precision were satisfactory. The estimated limits of detection and limits of quantification ranged from 0.01 to 0.1 mg/kg and from 0.02 to 0.3 mg/kg, respectively. The proposed procedure was found to be useful for the multiresidue analyses of pesticides in agricultural products for routine monitoring programs.     

Analysis for 2,3,7,8-tetrachlorodibenzofuran and 2,3,7,8-tetrachlorodibenzo-P-dioxin in a soot sample from a transformer explosion in Binghamton,New York

2,3,7,8-TCDF and 2,3,7,8-TCDD were found in a soot sample from a transformer explosion that occurred in an office building in Binghamton, New York. The isomer-specific analytical method was high-performance liquid chromatography, capillary gas chromatography and high-resolution mass spectrometry.     

Quantities of bisphenol a leached from plastic waste samples

To quantify the leaching of bisphenol A into water, various samples of plastic waste were cut into small pieces, soaked in water for two weeks at room temperature in the dark, and the concentration of bisphenol A in the water determined by gas chromatography/mass spectrometry (GC/MS). The amount of bisphenol A leached from the plastic wastes ranged from undetectable to 139 micrograms/g. The detection limit was 2 ng/g when 100 g of plastic waste was used. Polyvinyl chloride products yielded the highest concentrations because bisphenol A is used in its manufacture as a stabilizer.     

Separation of toxaphene by high resolution gas chromatography

A summary is given about the separation of toxaphenes by high resolution gas chromatography (HRGC). The suitability of different stationary phases for isomer and/or enantiomer-selective separations is compared. Multidimensional and tandem techniques are also presented. In addition, problems caused by thermal degradation in the injector and on the column are addressed. Furthermore, a brief survey is included about detection methods such as electron capture detection and different mass spectrometric methods.     

Isolation and identification of beta-nitrostyrene from smoked chicken

Extraction and identification of beta-nitrostyrene from smoked chicken is described. Commercially obtained smoked chicken was homogenised and extracted with chloroform-methanol (2:1). The extracts were fractioned by silicic acid column chromatography. The purified extract using thin-layer chromatography was identified by a colour reaction (this qualitative method for some nitrated compounds is developed this time), high pressure liquid chromatography and gas chromatography/mass spectrometry. The concentration of beta-nitrostyrene in the smoked chicken was 94 ppb. The average recovery of added beta-nitrostyrene was 107%. However, the toxicity of this material was not tested in the present paper.     

Potential antitermite compounds from Juniperus procera extracts

Thin layer chromatography (TLC) analysis revealed that destructive distillation of Juniperus procera tree gave ten major components, whereas Croton megalocarpus tree yielded five components. This was confirmed by gas chromatography (GC). The components were isolated by column chromatography and analysed using infrared, ultra-violet, visible and mass spectroscopy (MS) techniques. The whole extract was about 30.3% of the starting material (sawdust) and consisted of 77.5% water and 22.5% oily reddish-brown layer. The extracts had alcoholic and phenolic compounds together with acids. Cedrol, a tertiary tricyclic alcohol, was found to be in the greatest proportion in the oily layer. IR spectra with a peak beyond 3000 cm(-1), UV-VIS absorption maxima at 230 nm and mass spectra with m/e 204 suggested the presence of cedrene in the extract.     

Analysis of halogenated polycyclic aromatic hydrocarbons in urban air, snow and automobile exhaust

Urban air, snow and automobile exhaust samples were extensively cleaned up by open column liquid chromatography. The appropriate fractions were analysed for halogenated polycyclic aromatic hydrocarbons (XPAH) by gas chromatography/negative chemical ionization mass spectrometry (GC/NCIMS). XPAH were found in all three sample types. A urban air sample was found to contain chlorinated pyrenes, fluoranthenes and benzopyrene and brominated pyrenes and fluoranthenes. Furthermore, the concentration of 1-chloropyrene in that air sample was estimated to be 10 pg/m³. XPAH were also found in snow samples taken in the vicinity of a motor-way. Ethylene dibromide and ethylene dichloride, are probably the source of the halogen atoms in the XPAH detected in car exhaust.