Determination and speciation of arsenic in drinking water samples by X-ray spectrometry technique.

Arsenic is ranked as the first compound in the Substance Priority List 2023 by the Agency for Toxic Substances and Disease Registry (ATSDR). The most prominent entrance to the human body is through drinking water wherein the predominant species are arsenite and arsenate. The more toxic As(III) has rigorously threatened human health worldwide; hence, speciation and separation are the need of the hour. In this article, we have reported a simple method of arsenic speciation by wavelength dispersive X-ray fluorescence (WD-XRF) spectrometer. Valence to core (VtC) electronic transitions, i.e., AsKß2,5 fluorescence lines were used for arsenic speciation. This speciation study by WD-XRF entails direct measurement of activated alumina pellets containing arsenate and arsenite species adsorbed from water sample without separation of the trivalent and pentavalent species. This is the first report wherein the X-ray technique has been explored for speciation analysis of arsenic and the biggest advantage of the method lies in its applicability to direct analysis of synthesized nanotubes or other solid-phase extraction sorbents entrapping both the arsenic species. For determination of total arsenic using activated alumina as adsorbent, the most intense AsKα1,2 analytical lines were used and the instrumental limit of detection and the lower limit of quantification were 0.23 µg/L and 0.89 µg/L, respectively. For speciation, these limits were calculated to be 50 µg/L and 200 µg/L, respectively.

Primary congenital glaucoma: An iridotrabeculodysgenesis?

PURPOSE: To analyze primary congenital glaucoma (PCG) anterior chamber and angle anomalies over 360° as possible biomarkers of severity and prognosis. METHODS: A cross-sectional observational study was conducted analyzing anterior segment anomalies of PCG patients over 4 years of age who underwent trabeculectomy combined with trabeculotomy and age-matched controls using anterior segment optical coherence tomography (ASOCT), CASIA-2. Anterior iridotrabecular adhesions or anterior iris insertion was identified and quantified from the scleral spur using the iridotrabecular contact (ITC) index parameter as a surrogate. RESULTS: There was a variable but significantly increased anterior iridotrabecular adhesion on ITC index, ITC area, corneal volume, anterior chamber volume, iris volume, anterior chamber depth, and small/absent trabecular meshwork in PCG eyes compared to control eyes. In PCG eyes, anterior iridotrabecular adhesion had a positive correlation with pre-operative central corneal thickness (CCT) (r = 0.53, P = 0.02), review iris thickness (r = 0.4, P = 0.04), and ITC area (r = 0.85, P < 0.001). Review iris thickness had a negative correlation with pre-operative vertical cup-disc ratio (r = -0.51, P = 0.008). Iris hypoplasia with fewer or absent folds, collarette, pupillary ruff, and pupillary ruff to collarette distance was significantly different from controls. CONCLUSION: ASOCT in PCG eyes has shown that they have variable anterior iridotrabecular tissue adhesions, anomalous tissue/membranes in the angle, and iris hypoplasia correlating with pre-operative cup-disc ratio. These features could be used as gonioscopic and clinical biomarkers to assess the severity and prognosis of the disease. The presence of abnormal iris morphology and iridotrabecular tissue anomalies in PCG suggests that it is more than just isolated trabeculodysgenesis and is probably best considered as part of the anterior segment dysgenesis spectrum.

Rapid method of arsenic estimation in geological samples by WD-XRF using a novel concept of As-Pb concentration equivalence.

The presence of arsenic in ground waters of many countries has been a subject of global concern due to its toxicity. Primary sources of arsenic are geogenic, i.e. weathering and erosion of rocks and soils containing arsenic. This paper presents a rapid method for determination of arsenic in solid geological samples by wavelength dispersive X-ray fluorescence spectrometer. To achieve the best LLD (lower limit of detection), the most intense X-ray fluorescence line Kα1,2 is preferably used for determination of elemental concentrations because it pertains to the most probable transition. But the greatest challenge in arsenic estimation is the serious line overlap of AsKα1,2 lines with the equi-energy PbLα1,2 lines. By using the conventional line overlap correction methods, uncertainty and detection limits in arsenic determination are degraded to an unacceptable degree in samples which contains high lead and low arsenic concentrations. The proposed method bypasses the line overlap issue in employing a novel concept of arsenic-lead concentration equivalence factor for the cumulative peak of AsKα1,2 and PbLα1,2 fluorescence lines. The constancy of this factor for all geological matrices facilitates arsenic determination in samples universally irrespective of matrix elements. For the method validation, 22 international certified reference materials have been analysed and the results proved to be propitious wherein only one value out of 22 determinations showed relative error more than 20% of the certified values. This attests to the high accuracy of the proposed method which can effectively determine arsenic below 5 mg/kg in the presence of high lead concentration up to 1000 mg/kg.

Measurement Uncertainty and Validation for Quantitation of Salbutamol in Human Urine by Gas Chromatography-Tandem Mass Spectrometry.

A simple, rapid, sensitive and specific gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for quantitation of salbutamol in human urine using salbutamol-d3 as the internal standard. The processing of urines samples includes deconjugation with enzymatic hydrolysis, solid phase extraction procedure utilizing XAD2 column and liquid-liquid extraction accompanied by the derivatization by means of MSTFA/IODO-TMS/DTE mixture. The GC column was a HP Ultra-1 (17 m × 0.22 mm × 0.11 µm) used to separate the peak of interest. The data for GC-MS/MS were acquired and processed utilizing GC Labs Solution and Insight GCMS Software. The detection of spectra was performed on TQ 8050. This method included a chromatographic run of 13.67 min and the linearity was found over the concentration range of 250-2000 ng/mL with a regression coefficient (r2) of 0.99. The coefficient of variation for intra and interday assay precision was between 1.85 and 2.85% and the accuracy was between 95.50 and 107.04% for low quality control (QC), medium QC and high QC. The recovery was adequate to reliable detect the analyte at or below the level recommended by the World Anti-Doping Agency i.e., threshold 1000 ng/mL. The limit of detection and limit of quantification were found to be 10 and 100 ng/mL, respectively. The expanded measurement uncertainty (Uexp%) was found to be 8.28%.