A method for cancer elemental risk assessments in hookah: An example in two common types of traditional and flavored tobaccos in Iran.

AIM: This study aimed to compare the elemental composition of traditional and flavored hookah tobacco, with a focus on heavy metals. METHODS: We used inductively coupled plasma mass spectrometry (ICP-MS) to analyze the concentrations of 29 elements in the raw tobacco, tobacco ash, hookah water after smoking, and tobacco smoke. RESULTS: The results showed that the traditional tobacco had significantly higher metal concentrations than the flavored tobacco in all samples. Most of the toxic metals (more than 98 %) remained in the smoke of both types of tobacco. The tobacco and hookah smoke contained high levels of harmful metals that can pose health risks to hookah users.•ICP-MS provides a comprehensive analysis of multiple elements simultaneously and it allows for precise quantification of metal concentrations in different samples.•ICP-MS requires specialized equipment and trained personnel and it may not detect elements present in extremely low concentrations.

Portable smartphone-based colorimetric system for simultaneous on-site microfluidic paper-based determination and mapping of phosphate, nitrite and silicate in coastal waters.

Early and on-site detection of environmental contaminations and physicochemical parameters of seawater is increasingly preferred to guarantee hazard minimization in many settings. In this paper, we describe a combination of microfluidic paper-based sensors (µPADs) and an Android-based smartphone application (App) for simultaneous on-site quantification of phosphate (PO4-P), silicate (SiO3-Si) and nitrite (NO2-N) in coastal seawater samples. The developed App can on-site capture, process, and quantify the µPAD colorimetric outputs. This App uses an image processing algorithm for quantifying color intensity and relating the RGB components to the analyte concentrations. The GPS-tagged data can be stored on the smartphone or sent via social networks. The significant factors affecting the detection of the analytes were optimized using Box-Behnken design. Under optimized parameters, the proposed method presented the linear ranges between 5 and 100 µg L-1 for phosphate (R2 = 0.9909), 5 to 100 µg L-1 (R2 = 0.9819) for nitrite and 10 to 600 µg L-1 (R2 = 0.9933) for silicate. The LODs of the method for detection of phosphate, nitrite and silicate were 1.52 µg L-1, 0.61 µg L-1 and 3.74 µg L-1, respectively. The device was successfully used to simultaneous analyze and map the PO4-P, SiO3-Si and NO2-N of Bushehr coastal seawater samples (Iran). The results were confirmed by the lab-based conventional colorimetric methods using spectrophotometer.

Online Solid-Phase Extraction of Prometon and Prometryne Using MIL-101(Cr) as Sorbent before Gas Chromatographic Analysis: A Computational and Experimental Study and Comparison between Splitless and PTV Inlets.

In this study, prometryne and prometon were extracted and preconcentrated from aqueous media using an online solid-phase extraction-thermal desorption method coupled with gas chromatography-flame ionization detector (GC-FID), equipped with two different inlets: split and programmable temperature vaporizer (PTV). For this purpose, the applicability of Tenax and a metal-organic framework were investigated as solid-phase sorbents. Several effective parameters on the extraction efficiency, such as the amount of sorbent, sample volume, sample pH and thermal desorption procedure were optimized. The analytical performance of the proposed methods showed an excellent linear dynamic range for prometon and prometryne (0.25-100 µg/L) and relative standard deviation less than 4.01%. Moreover, the detection limits below 0.20 and 0.35 µg/L were determined for prometon and prometryne, respectively. Additionally, molecular docking was applied to clarify the adsorption nature and binding energy of MIL-101(Cr) toward the studied analytes, which indicated an appropriate correlation between computational and experimental results. Finally, the proposed method was developed and validated for prometon and prometryne and successfully applied for their extraction from agricultural water, spiked with prometon and prometryne through its direct introduction into the GC inlet.

Bottled water safety evaluations in IRAN: determination of bromide and oxyhalides (chlorite, chlorate, bromate) by ion chromatography.

Bottled water is most well liked within the world and attention is drawn due to its health issues. Oxyhalides is one amongst the foremost important by-products in bottled water which is produced by disinfection process such as "ozonation". International standards have been set and justified to permissible levels for chlorate, chlorite and bromate as 700, 700 and 10 µg/l. Thereafter, 168 samples of bottled water (mineral and drinking water) from Iran market obtained with the optimal working conditions and analyzed by ion chromatography (IC) with conductivity detector. The results actuated that 23 and 17 out of 168 samples as mineral and drinking water revealed bromate content in charge of the national permissible level, found as the mean level of 37.04 and 33.58 µg/l, respectively. According to risk assessment results, the average of hazard quotient (HQ) and lifetime excess cancer (ELCR) were calculated 6.955 × 10-3 and 0.25 × 10-3, respectively. Thereupon, it is indispensable to control as well as make consumers aware of oxyholides hazard especially bromate following governmental authorities with an insight to health sectors monitoring guidelines due to its obvious harmful effects and aspects on health issues.

Microextraction on a screw for determination of trace amounts of hexanal and heptanal as lung cancer biomarkers.

Solid phase microextraction on a screw was utilized for the extraction of hexanal and heptanal as lung cancer biomarkers from urine samples. Reduced graphene oxide (rGO) was coated on the surface of a stainless-steel set screw by electrophoretic deposition method. The screw was located inside a glass cover, and the created channel acted as the sample solution flow pass. A 5 mL glass syringe was connected to a syringe pump to direct the sample and the eluent through the channel. The extraction procedure was followed by gas chromatography/mass spectrometry (GC/MS) for separation and determination of the extracted aldehydes. The effective parameters on the extraction efficiencies of the analytes were identified and optimized. Under the optimal extraction conditions, the extraction time was as short as 10 min. The calibration curves indicated good linearity (R2 > 0.97) within the concentration range of 1.0-50 µg L-1. The obtained limits of detection (LODs) for hexanal and heptanal were down to 0.4 and 0.3 µg L-1, respectively. Considering the repeatability, simplicity, and eco-friendliness of this simple extraction method, it can be efficiently used for preconcentration of aldehydes in different samples.

Carbon fibers modified with polypyrrole for headspace solid phase microextraction of trace amounts of 2-pentyl furan from breath samples.

This study introduces micrometric carbon strands as a suitable fiber for headspace solid phase microextraction. Compared to previous supports, carbon fibers have mechanical flexibility, wide thermal expansion, and a large surface area, which is an important factor in headspace solid phase microextraction. The electrophoretic technique was applied to modify the surface of stainless steel and carbon fibers with polypyrrole. Modified carbon fibers were used for extraction of 2-pentylfuran (2-PF) as a model analyte from patients' breath and coffee samples. 2-PF belongs to the furan family, which was suggested as a biomarker for Aspergillus fumigatus and was classified as a possible carcinogen. 2-PF can be found in many heat-processed foods and drinks. The separation and detection of the analyte was performed by gas chromatography coupled to mass spectrometry. The effective factors in the extraction performance of the analyte by carbon fiber supports were investigated and optimized. Under optimized extraction conditions (temperature, 20 °C; time, 15 min; desorption temperature, 200 °C; desorption time, 2 min; salt concentration, 10% w/v; and stirring rate, 700 rpm), the limit of detection was calculated as 0.05 ng mL-1, whereas repeatability and fiber-to-fiber reproducibility (RSD %) was found to be in the range of 3.2-4.1%. The experimental results showed that the proposed fiber had greater extraction performance for 2-pentylfuran.

Easy Diagnosis of Jaundice: A Smartphone-Based Nanosensor Bioplatform Using Photoluminescent Bacterial Nanopaper for Point-of-Care Diagnosis of Hyperbilirubinemia.

One of the concerns of parents in the first days of their baby's birth is the baby's risk of jaundice/hyperbilirubinemia. This is because more than 60% of babies are born with jaundice that, if not timely diagnosed and subsequently treated, can lead to serious damage to their health. On the other hand, despite recent progress in sensor technology for clinical applications, the development of easy-to-use, cost-effective, sensitive, specific, and portable diagnostic devices, which use nontoxic and biodegradable materials in their design and fabrication, is still in high demand. Herein we present an easy-to-use, cost-effective, selective, nontoxic, and disposable photoluminescent nanopaper-based assay kit with a smartphone readout for easy diagnosis of neonatal jaundice through visual determination of Bilirubin (BR) in infants' blood samples. The developed BR assay kit comprises highly photoluminescent carbon dot (CD) sensing probes embedded in a bacterial cellulose (BC) nanopaper substrate (CDBN). The photoluminescence (PL) of the developed BR sensor is quenched in the presence of BR as a PL quencher and then selectively recovered upon blue light (λ = 470 nm) exposure, due to conversion of the unconjugated BR to the colorless oxidation products (non-PL quencher) through BR photoisomerization and photooxidation, that subsequently leads to selective PL enhancement of CDBN. The recovered PL intensity of the developed BR assay kit, which was monitored by integrated smartphone camera, was linearly proportional to the concentration of BR in the range of 2-20 mg dL-1. The feasibility of real application of the fabricated smartphone-based BR assay kit was also confirmed via comparing the results of our method with a clinical reference method for determination of BR concentration in infant's blood samples. With the advantages of nontoxicity and the extraordinary physicochemical properties of photoluminescent BC nanopaper as the sensing substrate, along with those of smartphone technology, we believe that our developed smartphone-based BR assay kit, as an easy-to-use, cost-effective (∼0.01 Euro per test), portable and novel sensing bioplatform, can be potentially exploited for sensitive, specific, rapid, and easy BR detection and jaundice diagnosis at the point of care (POC) and in routine clinical laboratories as well.

Preparation and evaluation of a deoxycholic-calix[4]arene hybrid-type receptor as a chiral stationary phase for HPLC.

We report the synthesis and enantioseparation characteristics of two novel covalently immobilized deoxycholic acid derivatives as chiral stationary phases for high-performance liquid chromatography. In the structure of the first stationary phase, the 3-position of deoxycholic acid is substituted with a 3,5-dinitrophenylcarbamoyl group and the second one has an additional calix[4]arene attached to the carboxylic group of the deoxycholic acid. The chromatographic performance of the stationary phases was evaluated with enantioseparation of N-(3,5-dinitrobenzoyl)-dl-leucine, N-(3,5-dinitrobenzoyl)-dl-valine, omeprazole, diclofop-methyl, dl-mandelic acid and (RS)-pregabalin. Comparison of the performance characteristics of the prepared chiral stationary phases provided evidence for the active involvement of the calix[4]arene unit in the chiral recognition process. Both stationary phases are chemically bonded to the silica and can be used in both normal-phase and reversed-phase modes.

Preparation and evaluation of a chiral HPLC stationary phase based on cone calix[4]arene functionalized at the upper rim with l-alanine units.

Here we report a new chiral stationary phase (CSP) immobilized on silica gel based on cone calix[4]arene functionalized at the upper rim with two l-alanine units as new chiral selector that has been used in high-performance liquid chromatography. The CSP was prepared by covalently bonding the allyl groups at the lower rim of calix[4]arene to silica gel by thiol-ene click chemistry reaction. Elemental analysis of the CSP showed that 120 µmol of chiral selector bonded per gram of silica gel. 1-Hexene was used for end-capping of unreacted mercapto groups on silica gel. Since the CSP is chemically bonded to the silica, it can be used in the normal-phase and reversed-phase mode and with halogenated solvents as mobile phases, if desired. The chromatographic performance of the CSP was evaluated in the enantioseparation of the 3,5-dinitrobenzoyl derivatives of some amino acids, diclofop-methyl and dl-mandelic acid.

In-tube magnetic solid phase microextraction of some fluoroquinolones based on the use of sodium dodecyl sulfate coated Fe3O4 nanoparticles packed tube.

In-tube magnetic solid phase microextraction (in-tube MSPME) of fluoroquinolones from water and urine samples based on the use of sodium dodecyl sulfate (SDS) coated Fe3O4 nanoparticles packed tube has been reported. After the preparation of Fe3O4 nanoparticles (NPs) by a batch synthesis, these NPs were introduced into a stainless steel tube by a syringe and then a strong magnet was placed around the tube, so that the Fe3O4 NPs were remained in the tube and the tube was used in the in-tube SPME-HPLC/UV for the analysis of fluoroquinolones in water and urine samples. Plackett-Burman design was employed for screening the variables significantly affecting the extraction efficiency. Then, the significant factors were more investigated by Box-Behnken design. Calibration curves were linear (R(2)>0.990) in the range of 0.1-1000µgL(-1) for ciprofloxacin (CIP) and 0.5-500µgL(-1) for enrofloxacin (ENR) and ofloxacin (OFL), respectively. LODs for all studied fluoroquinolones ranged from 0.01 to 0.05µgL(-1). The main advantages of this method were rapid and easy automation and analysis, short extraction time, high sensitivity, possibility of fully sorbent collection after analysis, wide linear range and no need to organic solvents in extraction.

Electrochemically controlled in-tube solid phase microextraction.

We report a new in-tube solid phase microextraction approach named electrochemically controlled in-tube solid phase microextraction (EC in-tube SPME). This approach, which combined electrochemistry and in-tube SPME, led to decrease in total analysis time and increase in sensitivity. At first, pyrrole was elctropolymerized on the inner surface of a stainless steel tube. Then, the polypyrrole (PPy)-coated in-tube SPME was coupled on-line to liquid chromatography (HPLC) to achieve automated in-tube SPME-HPLC analysis. After the completion of EC-in-tube SPME-HPLC setup, the PPy-coated tube was used as working electrode for uptake of diclofenac as target analyte. Extraction ability of the tube in presence and in absence of applied electrical field was investigated. It was found that, under the same extraction conditions, the extraction efficiency could be greatly enhanced by using the constant potential. Important factors are also optimized. The detection limit (S/N=3) and precision were 0.1 µg L(-1) and 4.4%, respectively.

Electrochemically controlled in-tube solid phase microextraction of naproxen from urine samples using an experimental design.

A new in-tube solid phase microextraction approach named electrochemically controlled in-tube solid phase microextraction (EC in-tube SPME) has been reported. In this approach, in which electrochemistry and in-tube SPME were combined, the total analysis time was decreased and the sensitivity was increased. After electropolymerization of pyrrole on the inner surface of a stainless steel tube, the polypyrrole (PPy)-coated in-tube SPME was coupled on-line to high performance liquid chromatography (HPLC) to achieve automated in-tube SPME-HPLC analysis. After the completion of the EC-in-tube SPME-HPLC system, the PPy-coated tube was used as a working electrode for the uptake of naproxen. It was found that the extraction efficiency could be significantly enhanced using the constant potential. Plackett-Burman design was employed for screening, to determine the variables significantly affecting the extraction efficiency. The significant factors were then optimized using a Box-Behnken design. The linear range and detection limit (S/N = 3) were 0.5-1000 and 0.07 µg L(-1), respectively. Urine samples were successfully analyzed by the proposed method.

Simultaneous determination of penicillin G salts by infrared spectroscopy: Evaluation of combining orthogonal signal correction with radial basis function-partial least squares regression.

In this study, a new method for the simultaneous determination of penicillin G salts in pharmaceutical mixture via FT-IR spectroscopy combined with chemometrics was investigated. The mixture of penicillin G salts is a complex system due to similar analytical characteristics of components. Partial least squares (PLS) and radial basis function-partial least squares (RBF-PLS) were used to develop the linear and nonlinear relation between spectra and components, respectively. The orthogonal signal correction (OSC) preprocessing method was used to correct unexpected information, such as spectral overlapping and scattering effects. In order to compare the influence of OSC on PLS and RBF-PLS models, the optimal linear (PLS) and nonlinear (RBF-PLS) models based on conventional and OSC preprocessed spectra were established and compared. The obtained results demonstrated that OSC clearly enhanced the performance of both RBF-PLS and PLS calibration models. Also in the case of some nonlinear relation between spectra and component, OSC-RBF-PLS gave satisfactory results than OSC-PLS model which indicated that the OSC was helpful to remove extrinsic deviations from linearity without elimination of nonlinear information related to component. The chemometric models were tested on an external dataset and finally applied to the analysis commercialized injection product of penicillin G salts.

Separation and preconcentration of cadmium ions using octadecyl silica membrane disks modified by methyltrioctylammonium chloride.

A simple and selective method for the determination of cadmium in water samples by FAAS after solid phase extraction has been developed. The method is based on the sorption of cadmium as CdI(4)(2-) on octadecyl silica membrane disks modified by cationic surfactant of methyltrioctylammonium chloride in the pH range of 1-8. The sorbed cadmium is then eluted with 10ml of 1moll(-1) nitric acid in ethanol and is measured by flame atomic absorption spectrometry. The influence of flow rates of eluent and sample solution, iodide concentration and amount of surfactant in retention and elution of cadmium from disks was also investigated. A preconcentration factor of 100 was achieved by passing 1000ml of sample through the membrane disk. The limit of detection (LOD) of cadmium was found to be 0.014ngml(-1). Precision at 2.5mugl(-1) was 1.2% (n=8). The method was successfully applied to the determination of cadmium in some natural water samples. The accuracy was assessed through recovery experiment, independent analysis by graphite furnace atomic absorption spectrometry, and analysis of certified reference waters.

Determination of residual solvents and investigation of their effect on ampicillin trihydrate crystal structure.

In the present work, the relationship between residual solvents concentration and ampicillin trihydrate crystals stability has been investigated. The amounts of residual solvents determined by GC, X-ray powder diffraction (XRPD) and Fourier transform infrared spectroscopy (FT-IR) were used for characterization of solid state. The obtained results have shown good relationship between concentration of methylene chloride (as a critical residue solvent) and degree of ampicillin trihydrate crystallinity. As with the increasing methylene chloride concentration in the sample the degree of crystallinity decreased after stability test. From this relationship, critical concentration of methylene chloride into the ampicillin trihydrate is obtained and the results can be used for improving the large-scale production of ampicillin trihydrate.