Detection Limit Of Method Research Articles

Determination of Levels of Selected Essential and Non Essential Metals in Mango (Mangifera indica L.) Cultivated in Wolaita Zone, Southern Ethiopia

Background: Mango (Mangifera indica L.) is one of the most important tropical fruits commercialized and consumed worldwide fresh or processed, having an attractive color and distinct taste and aroma. The main objective of this study is to determine the level of selected essential and non-essential metals in Mango. Methods: The levels of essential and non-essential metals were determined in mango (Mangifera indica L.) samples collected from four different sites (Boloso Bombe, Boloso Sore, Damot woyde and Humbo) in Wolaita Zone, Southern Ethiopia by flame atomic absorption spectrometry. A 0.5 g dried powdered mango sample was digested with 1 mL of nitric acid (HNO3), 3 mL of perchloric acid (HClO4) and 1 mL of hydrogen peroxide (H2O2) at 180°C for 2:00 hours. The study focused on two mango varieties, the Apple mango and the Keitt mango. Result: The metal contents in the apple mango in mg/kg were found in the following order: Mg (20.04-0.34) greater than Ca (1.49-6.78) greater than Zn (2.32-4.23) greater than Fe (2.77-2.85) greater than K (2.03-2.41) greater than Na (1.72-1.97) greater than Mn (0.47-1.36) mg/kg; and that of the Keitt mango samples in mg/kg were in the order of: Mg (2o.08_20.34) greater than Ca (0.95_5.84) greater than Zn (2.69_3.66) greater than Fe (2.69_2.90) greater than K (1.91_2.77) greater than Na (1.79_1.93) greater than Mn (0.38_0.72) mg/kg, respectively. The levels of Cd and Pb were below method detection limit. Analysis of variance (ANOVA) at 95% confidence level indicated that there is significant difference in the mean concentration of all metals between the four sample sites. There was good correlation between the levels of some metals (Mg, Ca, Zn, Fe K, Na and Mn) in both varieties of mango samples. From the results of this study it can be concluded that the studied mango varieties grown in the study area are good source of essential metals and free from the toxic metals: Cd and Pb.

Elemental Characterization of Ambient Particulate Matter for a Globally Distributed Monitoring Network: Methodology and Implications.

Global ground-level measurements of elements in ambient particulate matter (PM) can provide valuable information to understand the distribution of dust and trace elements, assess health impacts, and investigate emission sources. We use X-ray fluorescence spectroscopy to characterize the elemental composition of PM samples collected from 27 globally distributed sites in the Surface PARTiculate mAtter Network (SPARTAN) over 2019-2023. Consistent protocols are applied to collect all samples and analyze them at one central laboratory, which facilitates comparison across different sites. Multiple quality assurance measures are performed, including applying reference materials that resemble typical PM samples, acceptance testing, and routine quality control. Method detection limits and uncertainties are estimated. Concentrations of dust and trace element oxides (TEO) are determined from the elemental dataset. In addition to sites in arid regions, a moderately high mean dust concentration (6 μg/m3) in PM2.5 is also found in Dhaka (Bangladesh) along with a high average TEO level (6 μg/m3). High carcinogenic risk (>1 cancer case per 100000 adults) from airborne arsenic is observed in Dhaka (Bangladesh), Kanpur (India), and Hanoi (Vietnam). Industries of informal lead-acid battery and e-waste recycling as well as coal-fired brick kilns likely contribute to the elevated trace element concentrations found in Dhaka.

Sampling of atmospheric Hgo using home-made gold-coated sand sorbent prior to analysis by atomic absorption spectrometry

Gold-coated sand for amalgamation was synthesized and applied for the determination of mercury in ambient air using a home-made dual gold trap unit coupled to atomic absorption spectrometer. Gold-coated sand is prepared by chemical reduction of Au(III) solution with hydroxylamine depositing elemental gold on acid-etched sand. A home-made dual gold trap unit which focused time-resolved mercury trapped from the sampling/first trap provided an increase in sensitivity and reliability for the analysis of ultra-trace mercury in air was designed and tested. Instrumental detection and quantitation limits (IDL and IQL) of system were 3.9 and 13pg Hg, respectively. Method detection and quantitation limits (MLOD and MLOQ) of system were 0.04 and 0.13ngHg.m-3 for sampling flow rate of 200mL.min-1 and sampling time of 8 hours. Sampling system for gaseous elemental mercury was set up and cooperated with home-made desorption system were preliminarily applied for analysis of atmospheric mercury in samples collected at Hochiminh city University of Science. The atmospheric mercury concentrations were in range of 2.7 – 8.1ng Hg. m-3 which were comparable to Hg concentration found in other cities in the world.

Per- and polyfluoroalkyl substances in waterbird feathers around Poyang Lake, China: Compound and species-specific bioaccumulation

As a nondestructive means of environmental monitoring, bird feathers have been used to analyze levels of per- and polyfluoroalkyl substances (PFASs) in specific environments. In this study, feather samples from 10 waterbird species around Poyang Lake were collected, and a pretreatment method for PFASs in feathers was optimized. The results showed that a combined cleaning method using ultrapure water and n-hexane effectively removed external PFASs. Twenty-three legacy and emerging PFASs were identified in the feathers of waterbirds, of which hexafluoropropylene oxides (HFPOs), chlorinated polyfluoroalkyl ether sulfonates (Cl-PFESAs), and sodium p-perfluorinated noneoxybenzene sulfonate (OBS) were reported for the first time, with their concentrations ranging from 0.060–2.4 ng·g−1 dw, 0.046–30 ng·g−1 dw, and lower than the method detection limit to 30 ng·g−1 dw, respectively. Compound- and species-specific bioaccumulation of PFASs was observed in the feathers of different waterbird species, suggesting that different PFAS types can be monitored through the selection of different species. Moreover, the concentrations of most PFCAs (except perfluorobutyric acid), perfluorooctane sulfonate (PFOS), and perfluorooctane sulfonamide (FOSA) were significantly positively correlated with δ15N (p < 0.05), while the concentrations of HFPOs, Cl-PFESAs, and OBS had significant positive correlations with δ13C. This indicates that the bioaccumulation of legacy and emerging PFASs in waterbird feathers is affected by their trophic level, feeding habits, and foraging area.

Point-of-Use SERS Approach for Efficient Determination and Removal of Phthalic Acid Esters Based on a Metal-Organic Framework-Coated Melamine Sponge.

Phthalic acid esters (PAEs) are ubiquitous environmental contaminants, and their real-time monitoring and removal remain challenging. Herein, a point-of-use (POU) device integrating adsorption, surface-enhanced Raman spectroscopy (SERS), and removal strategy was developed and realized ultrafast on-site determination of PAEs and cleanup of them from water. A piece of flexible melamine sponge (MS) was coated with gold nanostars (AuNSs) and metal-organic frameworks (MOFs), thus obtaining SERS activity and adsorption capacity. Based on this multifunctional AuNSs@MOFs/MS composite, clear trends were observed between SERS signal intensity and concentration of di(2-ethylhexyl)phthalate (DEHP) and dibutyl phthalate (DBP). The method detection limits of DEHP and DBP were calculated to be 0.75 × 10-7 and 0.67 × 10-7 M in water, respectively, proving good sensitivity. Furthermore, this POU device exhibited satisfactory adsorption capacity (∼82.3 g/g for DBP and ∼90.0 g/g for DEHP), high adsorption efficiency (equilibrium in 100 s), and good regeneration capability (removal efficiency >70% after 5 cycles). The applicability of this device was verified by its good determination and removal performance in real environmental water matrices. The whole process could be completed within 5 min. This approach provides a new POU alternative for real-time monitoring and removal of PAEs in water.

Imaging flow cytometric detection of del(17p) in bone marrow and circulating plasma cells in multiple myeloma.

Detection of del(17p) in myeloma is generally performed by fluorescence in situ hybridization (FISH) on a slide with analysis of up to 200 nuclei. The small cell sample analyzed makes this a low precision test. We report the utility of an automated FISH method, called "immuno-flowFISH", to detect plasma cells with adverse prognostic risk del(17p) in bone marrow and blood samples of patients with myeloma. Bone marrow (n = 31) and blood (n = 19) samples from 35 patients with myeloma were analyzed using immuno-flowFISH. Plasma cells were identified by CD38/CD138-immunophenotypic gating and assessed for the 17p locus and centromere of chromosome 17. Cells were acquired on an AMNIS ImageStreamX MkII imaging flow cytometer using INSPIRE software. Chromosome 17 abnormalities were identified in CD38/CD138-positive cells in bone marrow (6/31) and blood (4/19) samples when the percent plasma cell burden ranged from 0.03% to 100% of cells. Abnormalities could be identified in 14.5%-100% of plasma cells. The "immuno-flowFISH" imaging flow cytometric method could detect del(17p) in plasma cells in both bone marrow and blood samples of myeloma patients. This method was also able to detect gains and losses of chromosome 17, which are also of prognostic significance. The lowest levels of 0.009% (bone marrow) and 0.001% (blood) for chromosome 17 abnormalities was below the detection limit of current FISH method. This method offers potential as a new means of identifying these prognostically important chromosomal defects, even when only rare cells are present and for serial disease monitoring.

4D-Printed Elution-Peak-Guided Dual-Responsive Monolithic Packing for the Solid-Phase Extraction of Metal Ions.

Four-dimensional printing (4DP) technologies are revolutionizing the fabrication of stimuli-responsive devices. To advance the analytical performance of conventional solid-phase extraction (SPE) devices using 4DP technology, in this study, we employed N-isopropylacrylamide (NIPAM)-incorporated photocurable resins and digital light processing three-dimensional printing to fabricate an SPE column with a [H+]/temperature dual-responsive monolithic packing stacked as interlacing cuboids to extract Mn, Co, Ni, Cu, Zn, Cd, and Pb ions. When these metal ions were eluted using 0.5% HNO3 solution as the eluent at a temperature below the lower critical solution temperature of polyNIPAM, the monolithic packing swelled owing to its hydrophilic/hydrophobic transition and electrostatic repulsion among the protonated units of polyNIPAM. These effects resulted in smaller interstitial volumes among these interlacing cuboids and improvements in the elution peak profiles of the metal ions, which, in turn, demonstrated the reduced method detection limits (MDLs; range, 0.2-7.2 ng L-1) during analysis using inductively coupled plasma mass spectrometry. We studied the effects of optimizing the elution peak profiles of the metal ions on the analytical performance of this method and validated its reliability and applicability by analyzing the metal ions in reference materials (CASS-4, SLRS-5, 1643f, and Seronorm Trace Elements Urine L-2) and performing spike analyses of seawater, groundwater, river water, and human urine samples. Our results suggest that this 4D-printed elution-peak-guided dual-responsive monolithic packing enables lower MDLs when packed in an SPE column to facilitate the analyses of the metal ions in complex real samples.

Evaluation of different QuEChERS-based methods for the extraction of 48 wastewater-derived organic contaminants from soil and lettuce root using high-resolution LC-QTOF with MRMHR and SWATH acquisition modes

The reuse of treated wastewater in agriculture is an important route of introducing a large number of organic contaminants into the agroecosystem. In this study, a modified QuEChERS-based approach was developed for rapid, simple, and simultaneous extraction of 48 organic wastewater-derived contaminants from soil and lettuce root. Twenty-two different (modification) scenarios of the known (or original) QuEChERS method have been tested, in order to obtain best and well-compromised recoveries for all target compounds for soil and roots. Finally, a common method was chosen for both matrices consisting of a single extraction step using EDTA-Mcllvaine buffer and the unbuffered Original QuEChERS salts. Method performance was accomplished by liquid chromatography coupled with high-resolution mass spectrometry on a QToF-MS system using two different acquisition modes, the ultra-fast high-resolution multiple reaction monitoring (MRMHR) mode and the innovative Sequential Window Acquisition of All Theoretical Fragment-Ion (SWATH) mode. Performance characterization was evaluated in terms of recovery, linearity, intra-day precision, method detection limits (MDLs), method quantification limits (MQLs), and matrix effect (ME). Recoveries in MRMHR mode ranged from 63 to 111% and 54 to 104% for lettuce root and soil, respectively, for most of compounds in MRMHR mode and from 56 to 121% and 54 to 104% for lettuce root and soil, respectively, for most of compounds in SWATH. Whereas, MQLs ranged from 0.03 to 0.92 ng g−1 in MRMHR and from 0.03 to 82 ng g−1 in SWATH for lettuce root, and from 0.02 to 0.44 ng g−1 in MRMHR and 0.02 to 0.14 ng g−1 in SWATH for soil. The method was then applied to follow the target compounds in soil and lettuce root, where the system lettuce-soil was irrigated with treated wastewater under real greenhouse conditions. Five and 17 compounds were detected in lettuce root and soil, respectively.Graphical

ANALYSIS OF HEAVY METAL CADMIUM (CD) CONTENT IN THE IE SEU’UM HIT WATER AREA IN ACEH BESAR

The Ie Seu'um hot springs area is located in Ie Seu'um Village, Mesjid Raya District, Aceh Besar Regency which has hot springs which are visited and used by the local community and tourists as a place for recreation with the family, a bathing place, and a place to boil food. Egg. The aim of this research is to determine and test heavy metals, namely Cadmium (Cd), which may be contained in the Ie Seu'um hot springs. The research used the AAS (Atomic Absorption Spectrophotometer) method. This research method uses a purposive sampling method, while the samples in this study were taken at spring points, namely places where people carry out egg-boiling activities and in holding tanks before the water flows into the bathing tubs. The results obtained for Cadmium (Cd) metal contained in hot springs (A) Ie Seu'um were &lt;0.0005#) and reservoirs (B) were 0.0005#). Based on the maximum standard for Cadmium (Cd) content according to the Regulation of the Minister of Health of the Republic of Indonesia Number 2 of 2023 in the Clean Water Requirements for heavy metals, this heavy metal does not exceed the threshold and is below the detection limit of the test method. It is hoped that the results of this research can become basic information for the public and tourists to always protect the ecosystem of the Ie Seu'um hot spring area and preserve local wisdom.

Occurrence and distribution of trisiloxane ethoxylates in citrus orchard soils in China: Analytical challenges

Trisiloxane ethoxylates (TSEOn) are widely used as agricultural surfactants due to their significant synergism with the active ingredients of pesticides, generally, including three typical end groups which are hydroxyl (TSEOn-H), methoxy (TSEOn-CH3), and acetoxy (TSEOn-COCH3), respectively. However, the potential ecotoxicological and endocrine-disrupting risks of TSEOn congeners have recently attracted ever-growing concern. Above all, there is limited research on the concentration levels of TSEOn in agroecosystems. This study, simultaneous analysis of 39 TSEOn oligomers in citrus orchard soils in China was implemented by the modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The method detection limits (MDLs) and the method quantification limits (MQLs) for TSEOn were 0.003–0.07 μg/kg and 0.01–0.20 μg/kg, respectively. The recoveries for TSEOn oligomers in soils ranged from 81 % ∼ 106 % with related standard deviations (RSDs) < 7 %. This newly developed UPLC-MS/MS method with high sensitivity and stability allows us to successfully trace the occurrence of TSEOn congeners in the citrus orchard soils from 3 provinces and 1 municipality in China. The detected concentrations of TSEOn-H oligomers in the sampled soils ranged from 0.02 to 0.288 μg/kg (dry weight). The congener profiles of TSEOn-H were dominated by TSEOn-H (n = 6– 8) in the soils. Additionally, the total concentrations of TSEOn-H congeners (ΣTSEOn-H) in the soils were in the range of 0.03 to 1.49 μg/kg. A comparison of ΣTSEOn-H distribution among the different citrus orchard soils indicated a higher level of ΣTSEOn-H in the soil samples collected from Zhejiang Province. Notably, TSEOn-CH3 or TSEOn-COCH3 oligomers were not detected in the tested soils. To the best of our knowledge, this is the first report on the occurrence and distribution of TSEOn congeners in agricultural soils.

Quantification of parabens in marine fish samples by a rapid, simple, effective sample preparation method.

Parabens (p-hydroxybenzoic acid esters) commonly used preservatives (in cosmetics, pharmaceuticals, and foods) can pose potential effects on environmental health. In this study, seven parabens were quantified in marine fish samples using an ultra-high performance liquid chromatography triple quadrupole mass spectrometer (UHPLC-MS/MS) system. Parabens in the fish samples were extracted and purified by a rapid, simple, and effective procedure comprising sample homogenization with solvent, solid-phase extraction clean-up, and solvent evaporation. Results demonstrated that the recoveries of seven compounds (with relative standard deviation < 15%) were 88-103% in matrix-spike samples and 86-105% in surrogate standards. The method detection limits and method quantification limits of seven parabens were 0.015-0.030 and 0.045-0.090ng/g-ww (wet weight), respectively. The optimized method was applied to measure the concentration of parabens in the 37 marine fish samples collected from Vietnam coastal waters. The concentration ranges of seven parabens found in round scad and greater lizardfish samples were 6.82-25.3ng/g ww and 6.21-17.2ng/g-ww, respectively. Among parabens, methylparaben accounted for the highest contribution in both fish species (43.2 and 44.9%, respectively). Based on the measured concentrations of parabens in marine fish samples, the estimated daily intake was calculated for children and adults with the corresponding values of 0.0477µg/kg/day and 0.0119µg/kg/day, respectively. However, the presence of parabens in Vietnamese marine fish may not pose a significant risk to human health.

Fluorescent Polymeric Sensor for Selective and Sensitive Detection of Cu(II) ions in Aqueous Medium

In our study, a selective and sensitive determination method was developed for Cu(II) ions by spectrofluorimetry. For this purpose, a polymeric membrane was prepared to determine Cu(II) ions by curing crosslinkers, functional monomers, and photoinitiators under UV light. The membrane was characterized, and the optimum conditions for determining Cu(II) ions were systematically investigated. The detection was performed at pH 5.0 in as little as 20 seconds at excitation and emission wavelengths of 376 nm and 455 nm, respectively. The linear range was 7.86.10-9-1.57.10-7 mol/L, and the method's detection limit was 2.24.10-9 mol/L. In addition, the sensor's repeatability, stability, and life were examined, and recovery studies were conducted. As a result, the developed method has been successfully applied to wastewater samples as a real sample. In addition, determining Cu(II) ions at low concentrations can be done quickly, reliably, and with high selectivity and sensitivity.

Chemical Vapor Generation Non-Dispersive Atomic Fluorescence Spectrometry Technique for the Determination of Arsenic, Antimony, Selenium, and Mercury in Geological Samples by One-Time Digestion

In this paper, a one-time digestion method for the determination of arsenic (As), antimony (Sb), selenium (Se), and mercury (Hg) in geological samples was established. The optimum digestion conditions were determined with aqua regia-hydrofluoric acid (HF)-H3BO3 as a complexing open system, and the contents of As, Sb, Se, and Hg in the same digestion solution were determined by chemical vapor generation non-dispersive atomic fluorescence spectrometry (CVG-AFS). For the determination of As, Sb, Se, and Hg, the method detection limits were 0.53 mg/kg, 0.047 mg/kg, 0.009 mg/kg, and 0.00047 mg/kg, respectively, Δ log C was -0.043–0.048, and the %RSD values were lower than 8.5%, performing with good accuracy and precision. This digestion method avoids the fractional processing of each element, simplifies the digestion steps, saves pretreatment time, and improves efficiency. The digestion method also showed wide applicability, high sensitivity, and low detection limits, and it can be used as a quick method for monitoring and controlling heavy metal pollution in large-scale geological samples.

Comparison of radium-226 separation methods based on chromatographic and extraction resins for its determination by ICP-MS in drinking waters.

Over the past century, human activities have contributed to the release of 226 Ra (t½ = 1,600 y) in the environment, increasing the potential risks for human exposure and thus prompting scientists to monitor it. Inductively coupled plasma mass spectrometry (ICP-MS) is an alternative to alpha-spectrometry for the quantification of 226 Ra. However, the performances of radioanalytical procedures are rarely compared in a rigorous framework, which means that researchers may choose one on subjective factors or guesses. This article compares five published methods for the separation and preconcentration of 226 Ra in drinking waters based on chromatographic and extraction resins prior to its analysis by ICP-MS. We evaluated the turnaround time, generated wastes, and final cost of each protocol as the economic aspect can be an important criterion when selecting a method, particularly for sustainable environmental monitoring. Our results showed that 226 Ra was successfully separated and preconcentrated, yielding recoveries ranging between 84% and 105%. Method detection and quantification limits of respectively 2-7fg L-1 (0.1-0.3 mBq L-1 ) and 6-24 fg L-1 (0.2-0.9 mBq L-1 ) were achieved when the separation method was coupled with ICP-MS. The turnaround times ranged between 6 and 21 hours, whereas the cost of the methods varied between 40 and 132 USD. This study highlights for the first time that methodologies recently published on the evaluation of 226 Ra levels in drinking water by ICP-MS have comparable figures of merit. Our results offer essential insights into the selection of the most suitable separation method.

Determination of cyclic volatile methylsiloxanes in sludge samples collected from To Lich River, Hanoi, Vietnam

Cyclic volatile methylsiloxanes (cVMSs) are synthesis chemicals used widely in consumer products such as building materials, households, electrical and medical devices, and personal care products. Due to being used in many applications, cVMSs are released into various micro-environments. Recently, the pollution level of cVMSs in the environment including sewage sludge has been gradually concerned. In this work, four typical cVMSs: hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylhexasiloxane (D6) were measured in 20 sludge samples collected from a sewage river (To Lich River) in Ha Noi metropolitan by using the gas chromatography-tandem mass spectrometry (GC-MS) method. The method detection limits (MDLs) and the method qualification limits (MQLs) of cVMSs in sewage sludge were a range of (1.20-3.00) ng/g-dw (dry weight) and (3.60-9.00) ng/g-dw, respectively. Recoveries of the surrogate compound (tetrakis-(trimethyl siloxane)-silane: M4Q) in blank and real samples were from (89.4 to 112) % (RSD: 9.2 %). The total concentrations of cVMSs in sewage sludge samples from To Lich River ranged from (260 to 13,800) ng/g-dw. Among the studied cVMSs, D5 was found at the highest levels in a range of (150-6,040) ng/g-dw. To our knowledge, this is the first report on the occurrence of cVMSs in sewage sludge samples in Ha Noi as well as Vietnam. The results indicate that the distribution of cVMSs in environments is significantly high and further studies should be conducted. ® 2023 Journal of Science and Technology - NTTU

Study on determination of PAEs in water samples by using solid phase extraction combined with gas chromatography-mass spectrometry

Phthalic acid diesters (PAEs) are industrial chemicals used as plasticizers in a variety of commercial products. Due to wide usage, PAEs have been found in various environments and their human exposure risks have also attracted a lot of concerns. However, little information about the distributions of PAEs in the water samples collected from Vietnam was reported. In this study, the method for the determination of nine typical PAEs in water samples by using the solid phase extraction (SPE) combined with gas chromatography-mass spectrometry (GC-MS) technique was optimized. The method detection limits (MDLs) and method quantitation limits (MQLs) of PAEs in water samples were in ranges of 0.2–0.4 ng/L and (0.6-1.2) ng/L, respectively. The recoveries of surrogate compounds in blank and real samples ranged from (74.8 to 93.9) %, with RSD &lt; 9.2 %. The calibration curve for all standards was linear over a concentration range of (1.0-1,000) ng/mL (with R2 ≥ 0.998). The total concentrations of PAEs measured in bottled water of six brands were ranged from 10.0 ng/L to 6,690 ng/L. Among the studied PAEs, di-(2-ethylhexyl) phthalate (DEHP) was found at the highest frequencies and concentrations. Overall, the distribution of PAEs in plastic bottled water is significantly lower than the permitted regulations (only with DEHP) in drinking water by the Ministry of Health of Vietnam in 2011. ® 2023 Journal of Science and Technology - NTTU

Development and optimization of a triple quadrupole ICP-MS-based system for the quantification of pre-concentrated gaseous elementary mercury.

Understanding the redox reactions and transformation rates of mercury (Hg) species in the environment is important for predicting future gaseous elemental Hg (Hg0) levels and assessing the impacts of anthropogenic Hg0 emissions on human health. Stable Hg isotope tracers are a promising tool for estimating Hg0 production rates; however, traditional analytical approaches for quantifying Hg0, such as atomic fluorescence spectroscopy or atomic absorption spectrometry, cannot differentiate between Hg isotopes, and alternative approaches, such as inductively coupled plasma mass spectrometry (ICP-MS) with a typical aqueous sample introductory system, have relatively higher detection limit of Hg. Here, we developed and evaluated a custom-made thermal desorption unit coupled directly to a triple quadrupole ICP-MS (ICP-QQQ) for the quantification of Hg0 pre-concentrated on Au traps. The performance of the system was validated with measurements of a Hg standard gas and of Hg0 generated from aqueous Hg standards. Using our system, we were able to detect ultra-trace amounts of Hg0 and obtain precise Hg isotope measurements with an analytical error of ≤ 3.5%. Calibration curves with superb linearity (r2 > 0.999) were obtained for the Hg concentration range of 0-300pg. The method detection limit was approximately 0.01-0.03pg of Hg. Using the latest ICP-QQQ instrument (Agilent 8900; Agilent Technologies Ltd.) was far superior to using a previous model (Agilent 8800), with the Agilent 8900 showing approximately five times higher sensitivity than the Agilent 8800 as well as the ability to precisely and simultaneously analyze up to five Hg isotopes by time-resolved analysis.

Fast New Method for Estimation of Captopril in Pure and Pharmaceutical Preparation by Reaction with Ammonium Ce (IV) Sulfate in Acid Medium

The determination of captopril (CAP) using a new continuous flow injection analysis (CFIA) method was given in this work CAP in its pure state and some of its pharmaceutical preparations. The technique can be described as simple, fast, sensitive, easy to operate, and low-cost. The CAP reacted with ammonium ceric(IV) sulfate (ACS)2(NH4 )2SO4Ce(SO4)2. 3 H2O in an acidic medium and the reaction led to the formation of a white, slightly yellowish precipitate. The formed precipitate was studied using Ayah 6S×1-ST-2D Solar cell-CFI Analyzer, a through the reflection of accident light on the surfaces of the precipitate particles at (0-1800), expressed as the response of the transducer measured in (mV). Some chemical and physical parameters were studied to provide the optimal conditions for the study. The calibration curve within the range of (0.07-3.0) mmol/L was linear, with a correlation coefficient (r) value equal to (0.9983), and the percentage value of linearity (R2%) was (99.65). The method's detection limit (L.O.D.) of the new method was 272.5 ng/25 µL; it was calculated by diluting the minimum concentration in the calibration curve gradually. RSD% was less than 0.2% for 0.9, 1.5, and 3.0 mmol/L concentrations of C.A.P. for n=8. The method was successfully applied to estimate C.A.P. in three pharmaceutical preparations, each produced by a different company. The new method was compared with the UV-Spectrophotometric method (classical method) at λmax= 207.2 nm by using the method of standard additions. Both the t-test and the F-test were conducted to ensure that there wasn't a significant difference between the new method and the conventional one. The results of both tests showed, at a confidence level of 95%, that there was no significant difference.

Optimization of the ultrasound-assisted extraction method for determining high production volume chemicals in fish liver and skin samples

The aquatic ecosystem is one of the most delicate environments, housing a diverse range of organisms, including fish, all of which are exposed to a wide variety of pollutants. The accumulation of these harmful substances in fish, which are part of the human diet, presents a significant health risk to humans. In our study, we have optimized an extraction technique to determine the presence of 25 high production volume chemicals in liver and skin samples taken from commonly consumed fish species. We have employed ultrasound-assisted extraction in conjunction with gas chromatography tandem mass spectrometry to achieve this goal. Apparent recoveries of the method ranged from 50% to 111% for both sample types with some exceptions such as most of the benzosulfonamides and benzothiazole. Additionally, the method's detection and quantification limits varied from 0.1 to 1.7 ng g−1 (dry weight, d.w) and 0.2–4.5 ng g−1 (d.w), respectively. Our investigation focused on three frequently consumed fish species in Tarragona: sea bass, sea bream, and turbot. Almost all of the samples we analysed contained traces of contaminants, with phthalates being the most commonly detected. The highest concentrations were observed for diethyl phthalate, with levels peaking at 8350 ng g−1 (d.w.). Organophosphate esters, such as triethyl phosphate and tributyl phosphate, also showed notable presence, with peak concentrations of 93.6 and 34.0 ng g−1 (d.w.), respectively.

Indicator-catalyst displacement assay for tandem detection and signal amplification of dimethoate organophosphate pesticide

This paper describes the chemosensing and catalytic amplification properties of [MnIII(TPP)(NCS)]–[PdII(DMSO)Cl2] (1, TPP = 5,10,15,20-tetraphenyl-21H,23H-porphine) for detecting the organophosphate pesticide dimethoate. Complex 1 selectively detects dimethoate, resulting in a visual color change from yellowish-brown to green with a UV–vis spectroscopic method detection limit (MDL) of 22.7 μM. This selectivity is attributed to the formation of a more stable PdII(dimethoate)2Cl2 adduct, resulting in the release of the colored MnIII(TPP)(NCS) unit from complex 1. Interestingly, the free PdII(dimethoate)2Cl2 released acts as a catalyst for the Heck coupling reaction of 5-diethylamino-2-iodo-phenyl ester (2), producing the highly fluorescent 7-diethylaminocoumarin (3). This catalytic process results in significant signal amplification, enhancing the original sensitivity by 25 times, with a spectrofluorimetric MDL of 0.9 μM. The proposed indicator-catalyst displacement assay successfully quantifies dimethoate concentrations in natural water samples, exhibiting good recoveries (92.5–108.1%) and low relative standard deviations (1.2–6.2%).