Chemical derivatization processes applied to amine determination in samples of different matrix composition

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A New Analyzer Based on Pellistor Sensor with Neural Network Data Postprocessing for Measurement of Hydrocarbons in Lower Explosive Limit Range

We present the results of a first stage of development work on a new type of analyzer for hydrogen and C1–C3 hydrocarbons concentration measurements in the lower explosive limit range, based on single pellistor sensor with artificial neural network data postprocessing

Automated analyser for monitoring the contents of hydrocarbons in gas emitted from exploratory bore-holes in the gas and oil industry

An automated analyser for total hydrocarbon contents and hydrocarbon composition (from methane to pentanes) was constructed and tested in both laboratory and field exploitation. It used two-channel analysis: continuous measurements of total hydrocarbon contents and periodic (90 or 150 s) composition analysis after separation of hydrocarbons on a gas chromatographic column. Flame ionization detectors were used in both channels. A simple 16-bit analogue-to-digital converter was used (4.8, practically four orders of magnitude), while the full measuring range (six orders of magnitude) was ensured by automatic dilution of the sample (or standard) with clean air. Full control of the operating (calibration/analyses) cycle was performed by microcomputer. An external programme, based on a computer provided with full information on the instrument operating conditions, presents the results of calibrations/analyses and enables them to be archived in a standard database used in the oil/gas drilling industry (N-LAB) by providing a suitable link. The instrument measuring range was 1 ppm to 100% with precision not worse than 5% at the detection limit. The analyser can operate autonomously for two months, recalibrating itself daily

Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection

An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer composed of formic acid and N,N-diisopropylethylamine at pH 4.5 in ultrasonic bath, extracts were cleaned up using Strata-X 33 μm Polymeric SPE column. The analytes were separated in gradient elution mode on C18 column and detected by mass spectrometer working with an electrospray source in negative ion mode. To confirm that analytical method is suitable for its intended use, several validation parameters, such as linearity, limits of detection and quantification, trueness and repeatibilty were evaluated. Calibration curves were linear within a studied range of concentrations (r2 ≥ 0.999) for six investigated sweeteners (CYC, ASP, ALI, DUL, NHDC, NEO). Three compounds (ACS-K, SAC, SCL) gave non-linear response in the investigated concentration range. The method detection limits (corresponding to signal-to-noise (S/N) ratio of 3) were below 0.25 μg mL−1 (μg g−1), whereas the method quantitation limits (corresponding to S/N ratio of 10) were below 2.5 μg mL−1 (μg g−1). The recoveries at the tested concentrations (50%, 100% and 125% of maximum usable dose) for all sweeteners were in the range of 84.2 ÷ 106.7%, with relative standard deviations <10% regardless of the type of sample matrix (i.e. beverage, yoghurt, fish product) and the spiking level. The proposed method has been successfully applied to the determination of the nine sweeteners in drinks, yoghurts and fish products. The procedure described here is simple, accurate and precise and is suitable for routine quality control analysis of foodstuffs

An evaluation of sucrose as a possible contaminant in e-liquids for electronic cigarettes by hydrophilic interaction liquid chromatography–tandem mass spectrometry

The influence of sucrose combustion products on smoking and nicotine addiction is still controversial because the presence of the sucrose may be treated as a source of aldehydes and organic acids. In e-liquids used as refills for electronic cigarettes, which are made primarily of poly(propylene glycol), glycerine and ethanol, sucrose may be present at trace levels, and its impact on mainstream smoke formation, and hence on human health and smoking/nicotine addiction is unknown. An analytical method was developed where high-performance liquid chromatography in hydrophilic interaction liquid chromatography mode and tandem mass spectrometry were used for fast and simple determination of sucrose and other saccharides in e-liquids for electronic cigarettes. Minimal effort was required in the sample preparation step, and satisfactory results were obtained, and the sample matrix had an insignificant impact. The chromatographic separation was done using an Ascentis Express OH5 column (150 mm × 2.1 mm, 2.7 μm). The coefficients of variation for within-day precision for three concentrations were 2.4 %, 1.6 % and 2.3 %, and the between-day coefficients of variation for a single concentration were 2.1 %, 2.5 % and 1.7 % measured on the next 3 days. The detection limit was 0.73 μg/g, and the sucrose content in e-liquids ranged from 0.76 to 72.93 μg/g among 37 samples. Moreover, with the method presented it is possible to determine the presence of other saccharides such as fructose, glucose, maltose and lactose. However, only sucrose was found in all samples of e-liquids. The proposed method is rapid, simple and reliable in terms of high-performance liquid chromatography coupled with tandem mass spectrometry

Impact of selected parameters of the fermentation process of wine and wine itself on the biogenic amines content: Evaluation by application of chemometric tools

The demand for safer foods has promoted more research into biogenic amines (BAs) over the past few years, however, there are still some questions that remain unanswered. Despite the fact that BAs are present in wine and can cause toxic effect to the body, a shared regulation limiting the amounts of BAs in wine is still lacking. A detailed understanding of their presence in wine is also important for the food trade sector. Therefore, the aim of this work was to determine the level of selected BAs in wine samples origin from Poland. Thereafter, the evaluation of correlation between concentration of BAs and selected parameters including pH, alcohol content and fermentation temperature by application of chemometric analysis was carried out. The BAs were determined by application of previously developed SPME-GC–MS methodology characterized by low detection limits ranged from 0.009 μg/L (tyramine) to 0.155 μg/L (histamine). Data obtained in this study show that none of the wine samples surpassed the toxic levels reported for BAs in the literature (the total BAs content was ranged from 7 to 2174 μg/L), therefore, these wines appear to be safe as regards the risk associated with the intake of potentially toxic BAs. Moreover, several correlations between occurrence, concentration of biogenic amines, important factors of winemaking process as well as physico-chemical parameters of wine were indicated. Even though information on BAs is currently not included in wine composition databases, information on their existence, distribution, concentration and knowledge of existing relationships between BAs and other wine parameters is crucial and may be useful for the food industry, health professionals and consumers

Automated analyser for monitoring trace amounts of volatile chloro-organic compounds in recirculated industrial water

An automated analyser of volatile chloro-organic compounds in water was constructed and tested using standard mixtures of dichloromethane and dichloroethane. It was based on continuous, countercurrent gas stripping of the liquid sample followed by periodic trapping of the analytes on two traps alternately connected to the bubbler outlet, and thermal desorption. When one trap performed adsorption, the other underwent desorption and cooling. Analytes were detected by an ECD detector. Integration, calibration, calculations and overall operating cycle control was performed by a microcomputer. The instrument guarantees a 0.02 ppm Cl (w/w) detection limit, a 0—2 ppm detection range and 2 months of autonomous operation. Results are reported every 13 min

Development of an analytical protocol for determination of cyanide in human biological samples based on application of ion chromatography with pulsed amperometric detection

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1-100 μg/L for urine, 5-100 μg/L for saliva, and 3-100 μg/L for sweat samples with determination coefficients (R)>0.992. Low detection limits (LODs) in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n=3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples