Background: Reliable values for method validity of organochlorine pesticides determination were investigated, in water by solid phase extraction and in sediment by Soxhlet extraction, followed by gas chromatography equipped with an electron capture detector. Organochlorine pesticides are categorized as Persistent Organic Pollutants. Hence, critical decisions to control exposure to these chemicals in the environment are based on their levels in different media; it is important to find valid qualitative and quantitative results for these components. In analytical chemistry, internal quality procedures are applied to produce valid logical results. Result: In this study, 18 organochlorine pesticides were targeted for analysis and determination in water and river sediment. Experiments based on signal-to-noise ratio, calibration curve slope and laboratory fortified blank methods were conducted to determine the limits of qualification and quantification. The data were compared with each other. The limitation values, following Laboratory Fortified Blank, showed significant differences in the signal-to-noise ratio and calibration curve slope methods, which are assumed in the results for the sample concentration factor to be 1,000 times in water and 10 times in sediment matrices. The method detection limit values were found to be between 0.001 and 0.005 μg/L (mean of 0.002 ± 0.001) and 0.001 and 0.005 μg/g (mean of 0.001 ± 0.001). The quantification limits were found to be between 0.002 and 0.016 μg/L (mean of 0.006 ± 0.004) and 0.003 and 0.017 μg/g (mean of 0.005 ± 0.003 μg/L) for water and sediment, respectively, based on the laboratory fortified blank method. Because of different slopes in the calibration methods, it was also found that the limitation values for some components from the internal standard were higher than from external standard calibration, because in the latter a factor for injection efficiency is applied for calibration. Conclusion: Technically, there are differentiations between detection limits for quality and quantity from component to component, resulting from noise, response factors of instruments and matrix interference. However, the calculation method is the cause of differentiation for each component of the different methods. The results show that for no matter what component, the relationship between these levels in different methods is approximately: Signal to Noise : Calibration Slope = 1:10. Therefore, due to different methods to determine LOD and LOQ, the values will be different. In the current study, laboratory fortified blank is the best method, with lower limitation values for Soxhlet and solid phase extraction of OCPs from sediment and water, respectively.

Background: In several years ago, infection with human papillomaviruses (HPVs), have been prevalent in the worlds especially HPV type 18, can lead to cervical cancer. Therefore, rapid, accurate, and early diagnosis of HPV for successful treatment is essential. The present study describes the development of a selective and sensitive electrochemical biosensor base on DNA, for early detection of HPV-18. For this purpose, a nanocomposite of reduced graphene oxide (rGO) and multiwalled carbon nanotubes (MWCNTs) were electrodeposited on a screen-printed carbon electrode (SPCE). Then, Au nanoparticles (AuNPs) were dropped on a modified SPCE. Subsequently, single strand DNA (ssDNA) probe was immobilized on the modified electrode. The link attached between AuNPs and probe ssDNA provided by l-cysteine via functionalizing AuNPs (Cys-AuNPs). The differential pulse voltammetry (DPV) assay was also used to electrochemical measurement. The measurement was based on the oxidation signals of anthraquninone-2-sulfonic acid monohydrate sodium salt (AQMS) before and after hybridization between the probe and target DNA. Results: The calibration curve showed a linear range between 0.01 fM to 0.01 nM with a limit of detection 0.05 fM. The results showed that the optimum concentration for DNA probe was 5 µM. The good performance of the proposed biosensor was achieved through hybridization of DNA probe-modified SPCE with extracted DNA from clinical samples. Conclusions: According to the investigated results, this biosensor can be introduced as a proprietary, accurate, sensitive, and rapid diagnostic method of HPV 18 in the polymerase chain reaction (PCR) of real samples.

A novel method for the rapid modification of fullerene for subsequent enzyme attachment to create a potentiometric biosensor is presented. Urease was immobilized onto the modified fullerene nanomaterial. The modified fullerene-immobilized urease (C₆₀-urease) bioconjugate has been confirmed to catalyze the hydrolysis of urea in solution. The biomaterial was then deposited on a screen-printed electrode containing a non-plasticized poly(n-butyl acrylate) (PnBA) membrane entrapped with a hydrogen ionophore. This pH-selective membrane is intended to function as a potentiometric urea biosensor with the deposition of C₆₀-urease on the PnBA membrane. Various parameters for fullerene modification and urease immobilization were investigated. The optimal pH and concentration of the phosphate buffer for the urea biosensor were 7.0 and 0.5 mM, respectively. The linear response range of the biosensor was from 2.31 × 10⁻³ M to 8.28 × 10⁻⁵ M. The biosensor’s sensitivity was 59.67 ± 0.91 mV/decade, which is close to the theoretical value. Common cations such as Na⁺, K⁺, Ca²⁺, Mg²⁺ and NH₄⁺ showed no obvious interference with the urea biosensor’s response. The use of a fullerene-urease bio-conjugate and an acrylic membrane with good adhesion prevented the leaching of urease enzyme and thus increased the stability of the urea biosensor for up to 140 days.

Integrating polypyrrole-cellulose nanocrystal-based composites with glucose oxidase (GOx) as a new sensing regime was investigated. Polypyrrole-cellulose nanocrystal (PPy-CNC)-based composite as a novel immobilization membrane with unique physicochemical properties was found to enhance biosensor performance. Field emission scanning electron microscopy (FESEM) images showed that fibers were nanosized and porous, which is appropriate for accommodating enzymes and increasing electron transfer kinetics. The voltammetric results showed that the native structure and biocatalytic activity of GOx immobilized on the PPy-CNC nanocomposite remained and exhibited a high sensitivity (ca. 0.73 μA·mM⁻¹), with a high dynamic response ranging from 1.0 to 20 mM glucose. The modified glucose biosensor exhibits a limit of detection (LOD) of (50 ± 10) µM and also excludes interfering species, such as ascorbic acid, uric acid, and cholesterol, which makes this sensor suitable for glucose determination in real samples. This sensor displays an acceptable reproducibility and stability over time. The current response was maintained over 95% of the initial value after 17 days, and the current difference measurement obtained using different electrodes provided a relative standard deviation (RSD) of 4.47%.