Validation of the procedure for the simultaneous determination of aflatoxins ochratoxin A and zearalenone in cereals using HPLC-FLD

Method validation for quantitative analysis of aflatoxins (AFs), ochratoxin A (OTA) and zearalenone (ZEA) in cereals using HPLC with fluorescence detector (FLD) is described. Mycotoxins were extracted with methanol : water (80 : 20) and purified with a multifunctional AOZ immunoaffinity column before HPLC analysis. The validation of the analytical method was performed to establish the following parameters: specificity, selectivity, linearity, limits of detection (LOD) and quantification (LOQ), accuracy, precision (within- and between-day variability), stability, robustness, measurement of performance, and measurement of uncertainty. Calibration curves were linear (r > 0.999) over the concentration range, from the LOQ to 26, 40 and 400 ng/g for AFs, OTA and ZEA, respectively. LOD and LOQ were 0.0125 and 0.05 ng/g for aflatoxin B1 (AFB1) and G1 (AFG1), 0.0037 and 0.015 ng/g for aflatoxin B2 (AFB2) and G2 (AFG2), as well as 0.05 and 0.2 ng/g for OTA and 0.5 and 2 ng/g for ZEA, respectively. The mean recovery values were 77-104% for different concentrations of AFs, OTA and ZEA in spiked cereal samples. Both intra- and inter-day accuracy and precision were within acceptable limits. This method was successfully applied for the simultaneous determination of mycotoxins for 60 cereal samples collected from Malaysian markets. Fifty per cent of the cereal samples were contaminated with at least one of these mycotoxins, at a level greater than the LOD. Only one wheat sample and two rice samples were contaminated with levels greater than the European Union regulatory limits for AFs and OTA (4 and 5 ng/g). The means and ranges of mycotoxins obtained for the cereal samples were 0.4 ng/g and 0.01-5.9 ng/g for total AFs; 0.18 ng/g and 0.03-5.3 ng/g for OTA; and 2.8 ng/g and 2.4-73.1 ng/g for ZEA, respectively. The results indicate that the method is suitable for the simultaneous determination of AFs, OTA and ZEA in cereals and is suitable for routine analysis

Optimization and validation of a HPLC method for simultaneous determination of aflatoxin B1, B2, G1, G2, ochratoxin A, and zearalenone using experimental design.

A reversed-phase HPLC optimization strategy is presented for investigating the separation and retention behavior of aflatoxin B 1, B 2, G 1, G 2, ochratoxin A and zearalenone, simultaneously. A fractional factorial design (FFD) was used to screen the significance effect of seven independent variables on chromatographic responses. The independent variables used were: (X1) column oven temperature (20-40°C), (X2) flow rate (0.8-1.2 ml/min), (X3) acid concentration in aqueous phase (0-2%), (X4) organic solvent percentage at the beginning (40-50%), and (X5) at the end (50-60%) of the gradient mobile phase, as well as (X6) ratio of methanol/acetonitrile at the beginning (1-4) and (X7) at the end (0-1) of gradient mobile phase. Responses of chromatographic analysis were resolution of mycotoxin peaks and HPLC run time. A central composite design (CCD) using response surface methodology (RSM) was then carried out for optimization of the most significant factors by multiple regression models for response variables. The proposed optimal method using 40°C oven temperature, 1 ml/min flow rate, 0.1% acetic acid concentration in aqueous phase, 41% organic phase (beginning), 60% organic phase (end), 1.92 ratio of methanol to acetonitrile (beginning) and 0.2 ratio (end) for X1-X7, respectively, showed good prediction ability between the experimental data and predictive values throughout the studied parameter space. Finally, the optimized method was validated by measuring the linearity, sensitivity, accuracy and precision parameters, and has been applied successfully to the analysis of spiked cereal samples

Multidetachment analogue models of fold reactivation in transpression : the NW Persian Gulf

Two deformation events have been documented in the NW Persian Gulf during the Late Cretaceous and the Late Cenozoic. The most distinctive feature in this part of the Persian Gulf is the reactivation of the Late Cretaceous NNE-SSW Arabian trending folds by NE-SW shortening during the Late Cenozoic Zagros orogeny. In general, if a set of folds with horizontal axes is shortened roughly parallel to its fold axis, a dome-basin fold interference pattern is produced. In the NW Persian Gulf, reactivation of some old folds occurred instead of a fold interference pattern. Reactivation may be influenced by the following factors: i) the presence of incompetent layers (i.e. evaporites), ii) a variable overburden, iii) basement faults, and iv) obliquity between the younger deformation shortening axis and fold axis. It is this last factor that we investigated by means of analogue modelling. The experimental apparatus is similar to that commonly used for experiments with brittle-ductile systems at the Laboratory of Experimental Tectonics of Géosciences Rennes. The model consisted of an alternation of ductile and brittle horizontal layers with a stratigraphy similar to the one found in the NW Persian Gulf. The model was deformed by two deformation events with an angle a between the two directions of shortening. After deformation, the resulting structure resembled a fold facing the static wall with internal thrust faults and detachment faults arranged into a geometry similar to a fish tail. In the second shortening event, the fold was reactivated without formation of an interference pattern. Moreover, the displacement on both the reactivated and newly formed faults varied between almost pure thrust faults for low a and oblique thrust faults with a strike-slip component for high a. The models suggest that the presence of incompetent layers plays an important role in fold reactivation and confirm that basement faults are not necessary

Synthetic and living micropropellers for convection-enhanced nanoparticle transport

Nanoparticles (NPs) have emerged as an advantageous drug delivery platform for the treatment of various ailments including cancer and cardiovascular and inflammatory diseases. However, their efficacy in shuttling materials to diseased tissue is hampered by a number of physiological barriers. One hurdle is transport out of the blood vessels, compounded by difficulties in subsequent penetration into the target tissue. Here, we report the use of two distinct micropropellers powered by rotating magnetic fields to increase diffusion-limited NP transport by enhancing local fluid convection. In the first approach, we used a single synthetic magnetic microrobot called an artificial bacterial flagellum (ABF), and in the second approach, we used swarms of magnetotactic bacteria (MTB) to create a directable “living ferrofluid” by exploiting ferrohydrodynamics. Both approaches enhance NP transport in a microfluidic model of blood extravasation and tissue penetration that consists of microchannels bordered by a collagen matrix.ISSN:2375-254

Renal clearable catalytic gold nanoclusters for in vivo disease monitoring

Ultra-small gold nanoclusters (AuNCs) have emerged as agile probes for in vivo imaging, as they exhibit exceptional tumour accumulation and efficient renal clearance properties. However, their intrinsic catalytic activity, which can enable increased detection sensitivity, has yet to be explored for in vivo sensing. By exploiting the peroxidase-mimicking activity of AuNCs and the precise nanometer size filtration of the kidney, we designed multifunctional protease nanosensors that respond to disease microenvironments to produce a direct colorimetric urinary readout of disease state in less than 1 h. We monitored the catalytic activity of AuNCs in collected urine of a mouse model of colorectal cancer where tumour-bearing mice showed a 13-fold increase in colorimetric signal compared to healthy mice. Nanosensors were eliminated completely through hepatic and renal excretion within 4 weeks after injection with no evidence of toxicity. We envision that this modular approach will enable rapid detection of a diverse range of diseases by exploiting their specific enzymatic signatures

Thermal modelling of gas generation and retention in the Jurassic organic-rich intervals in the Darquain field, Abadan Plain, SW Iran

The petroleum system with Jurassic source rocks is an important part of the hydrocarbons discovered in the Middle East. Limited studies have been done on the Jurassic intervals in the 26,500 km2 Abadan Plain in south-west Iran, mainly due to the deep burial and a limited number of wells that reach the basal Jurassic successions. The goal of this study was to evaluate the Jurassic organic-rich intervals and shale gas play in the Darquain field using organic geochemistry, organic petrography, biomarker analysis, and basin modelling methods. This study showed that organic-rich zones present in the Jurassic intervals of Darquain field could be sources of conventional and unconventional gas reserves. The organic matter content of samples from the organic-rich zones corresponds to medium-to-high-sulphur kerogen Type II-S marine origin. The biomarker characteristics of organic-rich zones indicate carbonate source rocks that contain marine organic matter. The biomarker results also suggest a marine environment with reducing conditions for the source rocks. The constructed thermal model for four pseudo-wells indicates that, in the kitchen area of the Jurassic gas reserve, methane has been generated in the Sargelu and Neyriz source rocks from Early Cretaceous to recent times and the transformation ratio of organic matter is more than 97%. These organic-rich zones with high initial total organic carbon (TOC) are in the gas maturity stage [1.5–2.2% vitrinite reflectance in oil (Ro)] and could be good unconventional gas reserves and gas source rocks. The model also indicates that there is a huge quantity of retained gas within the Jurassic organic-rich intervals

Qualitative and quantitative analysis of mycotoxins.

Mycotoxin toxicity occurs at very low concentrations, therefore sensitive and reliable methods for their detection are required. Consequently, sampling and analysis of mycotoxins is of critical importance because failure to achieve a suitable verified analysis can lead to unacceptable consignments being accepted or satisfactory shipments unnecessarily rejected. The general mycotoxin analyses carried out in laboratories are still based on physicochemical methods, which are continually improved. Further research in mycotoxin analysis has been established in such techniques as screening methods with TLC, GC, HPLC, and LC–MS. In some areas of mycotoxin method development, immunoaffinity columns and multifunctional columns are good choices as cleanup methods. They are appropriate to displace conventional liquid–liquid partitioning or column chromatography cleanup. On the other hand, the need for rapid yes/no decisions for exported or imported products has led to a number of new screening methods, mainly, rapid and easy-to-use test kits based on immuno-analytical principles. In view of the fact that analytical methods for detecting mycotoxins have become more prevalent, sensitive, and specific, surveillance of foods for mycotoxin contamination has become more commonplace. Reliability of methods and well-defined performance characteristics are essential for method validation. This article covers some of the latest activities and progress in qualitative and quantitative mycotoxin analysis

Recent progress in developments of membrane materials and modification techniques for high performance helium separation and recovery : a review

Helium is a valuable gas with unique properties and applications and still the prominent industrial source of helium is natural gas. Because of several advantages of membrane-based separation processes over conventional methods as well as the lack of a comprehensive scientific report, the present study aims to investigate the advances in design and modification of organic and inorganic membranes and materials including pure polymers, mixed matrix membranes, polymer blends, copolymers, ceramics as well as carbon molecular sieves for separation and recovery of helium from methane and nitrogen. In overall, inorganic membranes such as silica have shown good performance in helium separation, but production of such membranes has not yet become viable on the commercial scale. On the other hand, polymeric membranes are low-priced, but their performance is relatively low with much room for improvements. One of the most effective methods to enhance the performance of these membranes is synthesizing copolymer membranes consisting of alternatively flat and bulky segments. Also, alternations in the membrane configurations as well as hybridization of membranes with cryogenic and pressure swing adsorption processes are among the valuable options for optimizing techno-economical viability of helium separation and purifcation

Multidetachment analogue models of fold reactivation in transpression : the NW Persian Gulf

Two deformation events have been documented in the NW Persian Gulf during the Late Cretaceous and the Late Cenozoic. The most distinctive feature in this part of the Persian Gulf is the reactivation of the Late Cretaceous NNE-SSW Arabian trending folds by NE-SW shortening during the Late Cenozoic Zagros orogeny. In general, if a set of folds with horizontal axes is shortened roughly parallel to its fold axis, a dome-basin fold interference pattern is produced. In the NW Persian Gulf, reactivation of some old folds occurred instead of a fold interference pattern. Reactivation may be influenced by the following factors: i) the presence of incompetent layers (i.e. evaporites), ii) a variable overburden, iii) basement faults, and iv) obliquity between the younger deformation shortening axis and fold axis. It is this last factor that we investigated by means of analogue modelling. The experimental apparatus is similar to that commonly used for experiments with brittle-ductile systems at the Laboratory of Experimental Tectonics of Géosciences Rennes. The model consisted of an alternation of ductile and brittle horizontal layers with a stratigraphy similar to the one found in the NW Persian Gulf. The model was deformed by two deformation events with an angle a between the two directions of shortening. After deformation, the resulting structure resembled a fold facing the static wall with internal thrust faults and detachment faults arranged into a geometry similar to a fish tail. In the second shortening event, the fold was reactivated without formation of an interference pattern. Moreover, the displacement on both the reactivated and newly formed faults varied between almost pure thrust faults for low a and oblique thrust faults with a strike-slip component for high a. The models suggest that the presence of incompetent layers plays an important role in fold reactivation and confirm that basement faults are not necessary