Application of Routine Analysis Procedures to a Direct Mass Spectrometry Technique: Selected Ion Flow Tube Mass Spectrometry (SIFT-MS)

In recent years the environmental and human health impacts of volatile organic compounds (VOCs) have become more apparent, resulting in increased analysis demand. The gold-standard chromatographic techniques continue to be employed for most laboratory analyses. However, they have made only modest gains in productivity over the years, and these gains are primarily due to automated sample preparation and injection. Alternatively, significant productivity gains for VOC analysis through faster sample analysis and reduced instrument maintenance could be achieved by adopting direct mass spectrometry techniques such as selected ion flow tube mass spectrometry (SIFT-MS). This article demonstrates that routine analysis techniques such as quality control checks, method validation, the method of standard additions, and internal standards are readily applied to SIFT-MS, simplifying adoption of the technique. In addition, workflows for analysis of chromatographically challenging species are simplified by using SIFT-MS. Sample throughputs are increased two- to 25-fold depending on the analytical procedure.

A Simple Distance Paper-Based Analytical Device for the Screening of Lead in Food Matrices

A simple and rapid distance paper-based analytical device (dPAD) for the detection of lead (Pb) in foods is proposed herein. The assay principle is based on competitive binding between carminic acid (CA) and polyethyleneimine (PEI) to Pb in a food sample. The paper channels were pre-immobilized with PEI, before reacting with a mixture of the sample and CA. Pb can strongly bind to the CA; hence, the length of the red color deposition on the flow channel decreased as a lower amount of free CA bound to PEI. The dPAD exhibited good linear correlation, with ranges of 5–100 µg·mL−1 (R2 = 0.974) of Pb. Although, the limit of detection (LOD) of this platform was rather high, at 12.3 µg·mL−1, a series of standard additions (8.0, 9.0, and 10.0 µg·mL−1) can be used to interpret the cutoff of Pb concentrations at higher or lower than 2 µg·mL−1. The presence of common metal ions such as calcium, magnesium, nickel, and zinc did not interfere with the color distance readout. The validity of the developed dPAD was demonstrated by its applicability to screen the contamination of Pb in century egg samples. The results obtained from the dPAD are in accordance with the concentration measured by atomic absorption spectroscopy (AAS) (n = 9). In conclusion, this proposed dPAD, combined with the standard addition method, could be applied for screening Pb contamination in food matrices. This platform is, therefore, potentially applicable for field measurements of Pb in developing countries, because it is cheap and rapid, and it requires no significant laborious instruments.

Multilinear Mathematical Separation in Chromatography

Chromatography is a powerful and generally applicable method for the analytical separation and quantification of the chemical constituents in complex mixtures because chromatographic separation can provide high selectivity by isolating all analytes from interferences. Multiway analysis based on the multilinear model is an increasingly widely used method for interference-free and fast determination of the chemical constituents also in complex mixtures because multilinear mathematical separation can provide high selectivity by extracting the pure signal of the analyte from the mixed signal of a real sample. By combining chromatographic separation with mathematical separation, multiway calibration method, multiway standard additions method, and multiway internal standard method can be established. Chromatography assisted by multiway analysis can reduce the requirements for complete chromatographic separation, save elution time, and decrease the consumption of the mobile phase, particularly when the peak coelution problem is difficult to solve. This review presents the fundamentals and analytical applications of multilinear mathematical separation in chromatography.

Comparative characterization of different kinds of chromatographic quantification using the double standard addition method

Different algorithms for processing the quantitative gas chromato­gra­­phic ana­lysis data using the double standard addition method are compared for their accuracy. Three principal approaches are possible for such processing: I – simple comparison of values determined by sing­le and double standard additions, II – approximation of «peak area of ana­lyte» (S) – «mass of standard addition» (madd) depen­den­ce by the least squa­res method [linear reg­res­sion, m(S)], and III – independent quantification of analyte with both standard additi­ons follo­wed by the linear extrapolation of two sub-results on the so-cal­led «zero standard addi­tion», mx(madd ® 0). It is concluded that the quantitation results obtained using the various modes of the method are comparable in accuracy, but somewhat underestimated relative to the specified amounts of analytes. The principal reason of such systematic errors is the eva­po­ration of the solvent during the successive injecting of the same samples into the gas chroma­to­graph. Due to this reason the peak are­as, measured after the standard addition, appear to be slight­­ly increased and this leads to the systematic underestimation of the results. The second (less impor­tant) factor is the small increa­se of the samp­le volumes due to the addition of the compo­nents to be determined. It is confirmed that the systematic errors of different modes of standard addition are not exceeding the values of their random uncertainties. The op­ti­mal results (considering their signs of deviations) are provided using the double standard addition method with extrapolation of sub-results on «zero standard addition». In order to exclude the possible influence of «human factor» (increasing the re­sults precision during the series of analyses of similar samples due to the rising experience of analytical chemists) all parallel measurements have been per­for­med by bachelor students of the Chemistry Ins­titute of the St. Petersburg State University in the course of their laboratory practical works in chromatography. Such organization of experiments increases their credibility as it excluded the dependence of the results on the qualification of chemists.

Determination of Bi in complex oxide samples by atomic absorption spectrometry by using ordinary acetylene – air flame atomization

In the present work the air/acetylene flame atomic absorption spectrometry was used for bismuth determination in complex oxides. Interference studies were carried out, and interference with vanadium and molybdenum was detected. The method of standard additions and traditional calibration curve method were used. Calibration and standard addition curves were fitted with linear and polynomial functions. It was shown that using polynomial function gives better results for the standard additions method for determination of bismuth by acetylene/air flame atomic absorption spectrometry. The calibration curve method was shown to be correct at low ( 10mg/L) concentration of an interferent.

Flow Injection–Indirect Spectrophotometry for Hydroquinone Analysis Based on the Formation of Iron(II)-Phenanthroline Complex

Hydroquinone is an organic antioxidant widely used for skin lightening products which can cause negative impact in excessive use. This study is focused on the development of fast method for the determination of hydroquinone using flow injection-indirect spectrophotometry based on the formation of red complex iron(II)-phenanthroline. In this method, hydroquinone reduced iron(III) to iron(II) which in the presence of phenanthroline formed iron(II)-phenanthroline complex detected at maximum wavelength of 510 nm. The common operational and chemical conditions were optimized and the effect of several interfering compounds was also studied to achieve the highest sensitivity with acceptable analysis time. The optimum method performance was obtained under the conditions of 100 µL sample volume, 50 cm mixing coil-1and 75 cm mixing coil-2, 5 ml/min flow rate, 100 mgL-1 Iron(III) concentration, and 0.15 % phenanthroline. Under these conditions the proposed FI-spectrophotometry gave results to linear calibration over the concentration range from 2-100 mgL-1 (y = 0.028x and R2 of 0.999). The method was not interfered in the presence of vitamin C 1 mgL-1 and resorcinol up to 10 mgL-1. However, the higher concentration of vitamin C ≥10 ppm and resorcinol ≥ 20 ppm gave significant error of measurements. Method validation using standard additions gave results to average recovery value of 97.02 %, which indicates that the FI-spectrophotometry method can be used as an alternative method for determining hydroquinone in cosmetic.