Neonicotinoids Detection by new LC-MS/MS Method in Romanian Surface Waters

2017 ◽  
Vol 68 (8) ◽  
pp. 1716-1722 ◽  
Author(s):  
Vasile Ion Iancu ◽  
Toma Galaon ◽  
Marcela Niculescu ◽  
Carol Blaziu Lehr
Keyword(s):  
Surface Water ◽  
Surface Waters ◽  
Water Samples ◽  
Solid Phase ◽  
Monitoring Program ◽  
Danube River ◽  
Limit Of Quantification ◽  
Neonicotinoid Insecticides ◽  
Relative Standard ◽  
Surface Water Samples

Increasing and widespread use of neonicotinoid insecticides in all world, together with their highly toxicity to invertebrates and environmental persistence mean that surface waters need to be monitored for these compounds. In the 2015, neonicotinoid insecticides have been incorporated in the watch list of substances for a European Union monitoring program (495/2015/ EU). A new method using automated solid phase extraction (SPE) with polymeric cartridges (OASIS HLB) followed by LC-MS/MS provided good separation of the most common neonicotindoid compounds. The method was developed for the determination of four neonicotinoid insecticides (nitenpyram, thiamethoxam, clothianidin, acetamiprid) in surface water with low limit of quantification (0.3-0.9 ng/L, nanograms per liter). Recoveries in surface water samples fortified at 200 ng/L for each compound ranged from 71.4 to 109.9 %; relative standard deviation ranged from 4 to 9%. The method was applied to water samples from four streams in Romania, Danube River and its tributaries (Arges River, Jiu River, and Olt River). The surface water samples were found to be contaminated clothianidin (1.08-6.4 ng/L) and by thiamethoxam (1.1-3.8ng/L). The highest concentrations were recorded in Danube River in Oltenita point (6.4ng/L) and in Gura-Vaii point (5.5ng/L). The concentration of acetamiprid and nitenpyram were situated below limit of quantification in all samples.

scholarly journals Development of Surface Molecularly Imprinted Polymers as Dispersive Solid Phase Extraction Coupled with HPLC Method for the Removal and Detection of Griseofulvin in Surface Water

2019 ◽  
Vol 17 (1) ◽  
pp. 134 ◽  
Author(s):  
Kamran Bashir ◽  
Zhimin Luo ◽  
Guoning Chen ◽  
Hua Shu ◽  
Xia Cui ◽  
...  
Keyword(s):  
Surface Water ◽  
Solid Phase Extraction ◽  
Molecularly Imprinted Polymers ◽  
Water Samples ◽  
Solid Phase ◽  
Phase Extraction ◽  
Dispersive Solid Phase Extraction ◽  
Molecularly Imprinted ◽  
Imprinted Polymers ◽  
Surface Water Samples

Griseofulvin (GSF) is clinically employed to treat fungal infections in humans and animals. GSF was detected in surface waters as a pharmaceutical pollutant. GSF detection as an anthropogenic pollutant is considered as a possible source of drug resistance and risk factor in ecosystem. To address this concern, a new extraction and enrichment method was developed. GSF-surface molecularly imprinted polymers (GSF-SMIPs) were prepared and applied as solid phase extraction (SPE) sorbent. A dispersive solid phase extraction (DSPE) method was designed and combined with HPLC for the analysis of GSF in surface water samples. The performance of GSF-SMIPs was assessed for its potential to remove GSF from water samples. The factors affecting the removal efficiency such as sample pH and ionic strength were investigated and optimized. The DSPE conditions such as the amount of GSF-SMIPs, the extraction time, the type and volume of desorption solvents were also optimized. The established method is linear over the range of 0.1–100 µg/mL. The limits of detection and quantification were 0.01 and 0.03 µg/mL respectively. Good recoveries (91.6–98.8%) were achieved after DSPE. The intra-day and inter-day relative standard deviations were 0.8 and 4.3% respectively. The SMIPs demonstrated good removal efficiency (91.6%) as compared to powder activated carbon (67.7%). Moreover, the SMIPs can be reused 10 times for water samples. This is an additional advantage over single-use activated carbon and other commercial sorbents. This study provides a specific and sensitive method for the selective extraction and detection of GSF in surface water samples.

scholarly journals Concentration and Detection of Cryptosporidium Oocysts in Surface Water Samples by Method 1622 Using Ultrafiltration and Capsule Filtration

2001 ◽  
Vol 67 (3) ◽  
pp. 1123-1127 ◽  
Author(s):  
Otto D. Simmons ◽  
Mark D. Sobsey ◽  
Christopher D. Heaney ◽  
Frank W. Schaefer ◽  
Donna S. Francy
Keyword(s):  
Surface Water ◽  
Surface Waters ◽  
Hollow Fiber ◽  
Water Samples ◽  
Environmental Protection Agency ◽  
Fluorescent Antibody ◽  
Immunomagnetic Separation ◽  
Recovery Rates ◽  
Microscopic Evaluation ◽  
Surface Water Samples

ABSTRACT The protozoan parasite Cryptosporidium parvumis known to occur widely in both source and drinking water and has caused waterborne outbreaks of gastroenteritis. To improve monitoring, the U.S. Environmental Protection Agency developed method 1622 for isolation and detection of Cryptosporidium oocysts in water. Method 1622 is performance based and involves filtration, concentration, immunomagnetic separation, fluorescent-antibody staining and 4′,6-diamidino-2-phenylindole (DAPI) counterstaining, and microscopic evaluation. The capsule filter system currently recommended for method 1622 was compared to a hollow-fiber ultrafilter system for primary concentration of C. parvum oocysts in seeded reagent water and untreated surface waters. Samples were otherwise processed according to method 1622. Rates of C. parvumoocyst recovery from seeded 10-liter volumes of reagent water in precision and recovery experiments with filter pairs were 42% (standard deviation [SD], 24%) and 46% (SD, 18%) for hollow-fiber ultrafilters and capsule filters, respectively. Mean oocyst recovery rates in experiments testing both filters on seeded surface water samples were 42% (SD, 27%) and 15% (SD, 12%) for hollow-fiber ultrafilters and capsule filters, respectively. Although C. parvum oocysts were recovered from surface waters by using the approved filter of method 1622, the recovery rates were significantly lower and more variable than those from reagent grade water. In contrast, the disposable hollow-fiber ultrafilter system was compatible with subsequent method 1622 processing steps, and it recovered C. parvum oocysts from seeded surface waters with significantly greater efficiency and reliability than the filter suggested for use in the version of method 1622 tested.

scholarly journals Occurrence and Distribution of Pharmaceuticals and their Transformation Products in Luxembourgish Surface Waters

2021 ◽  
Author(s):  
Randolph Singh ◽  
Adelene Lai ◽  
Jessy Krier ◽  
Todor Kondić ◽  
Philippe Diderich ◽  
...  
Keyword(s):  
Surface Water ◽  
Surface Waters ◽  
Water Samples ◽  
Transformation Products ◽  
Computational Tools ◽  
Data Files ◽  
Surface Water Samples

<p>This pre-print describes the analysis of pharmaceuticals and their transformation products in surface water samples collected in Luxembourg from 2019 to 2020. Details of the experimental and computational tools and workflows used are fully described in the manuscript. Links to the suspect lists, codes used, and data files are also provided.</p>

scholarly journals DISTRIBUTION OF CHEMICAL ELEMENTS IN SURFACE WATERS FROM THE CRNA RIVER BASIN, REPUBLIC OF MACEDONIA

2018 ◽  
Vol 39 (1) ◽  
pp. 31 ◽  
Author(s):  
Dimitri Tomovski ◽  
Trajče Stafilov ◽  
Robert Šajn ◽  
Katerina Bačeva Andonovska
Keyword(s):  
Surface Water ◽  
Surface Waters ◽  
Water Samples ◽  
Inductively Coupled Plasma ◽  
Chemical Elements ◽  
Emission Spectrometry ◽  
Anthropogenic Influence ◽  
Mean Values ◽  
Republic Of Macedonia ◽  
Surface Water Samples

An investigation of the distribution of 23 chemical elements (Ag, Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sr, V and Zn) in surface water samples from the entire basin of the Crna River, Republic of Macedonia, was carried out. In total 31 water samples were collected, from which 8 samples from the Crna River and 4 samples from four main tributaries of Crna River in the Pelagonia Valley (Blato, Prilepska Reka, Dragor and Jelaška Reka). Also, surface water samples were collected from 3 locations in the Tikveš Lake, 8 locations from the Majdanska River and river of Blašnica before its inflow into the Tikveš Lake and from 7 locations of the lower course of the Crna River after the dam of Tikveš Lake until its inflow into the river of Vardar. Determination of the concen-tration of the investigated elements was performed by using atomic emission spectrometry with inductively coupled plasma (ICP-AES). All data obtained for the analyzed samples were statistically processed using software Stat Soft 11.0 where the descriptive statistical analysis of the value for the concentration of the elements was performed. The maps of spatial distribution of the concentration for each element and a histograms for the representation of elements with mean values of the concentrations by regions, were also prepared. The obtained results show that the concentration of investigated element are mainly followed the lithology of the region. However, higher concentrations of arsenic were found in the water samples from the river of Blašnica which is a result of anthropogenic influence from the abounded Allchar mine on the Kožuf Mountain. Also, the increased concentrations of nickel were found in the samples from the lower couse of the Crna River after the dam of Tikveš Lake due to the anthropogenic influence from the ferronickel smelter plant Feni Industry, which can influence the quality parameters of surface waters.

scholarly journals Chemical Quality of Surface Water of Bhola Sadar Upazila in Bangladesh for Irrigation, Aquaculture, Drinking and Livestock Consumption

2015 ◽  
Vol 6 (1) ◽  
pp. 131-140
Author(s):  
MF Karim ◽  
MW Zaman ◽  
R Sultana ◽  
MU Nizam ◽  
MR Kamruzzaman
Keyword(s):  
Surface Water ◽  
Surface Waters ◽  
Water Samples ◽  
Pond Water ◽  
Magnesium Content ◽  
Low Salinity ◽  
Quality Of Water ◽  
Hard Limit ◽  
Surface Water Samples

A study was carried out with 25 pond water samples of Bhola Sadar Upazila to assess the quality of surface water for irrigation, aquaculture, drinking and livestock consumption. Chemical analyses of different parameters were done to assess the quality of water. All of the water samples showed slightly acidic in nature. Sixteen surface water samples were not suitable for drinking and aquaculture in respect of pH (pH <6.5). Electrical conductivity (EC) categorized the waters as “low salinity” (C1) to “medium salinity” (C2) class for irrigation. With respect to total dissolved solids surface waters were within “highest desirable limit” for drinking and irrigation and suitable for livestock consumption and aquaculture. Calcium and Magnesium content rated the samples as “maximum permissible” and “highest desirable” limit for drinking. All the samples were suitable for drinking in case of Na and K, 21 samples were not suitable for aquaculture due to higher (>5.0 mg L-1) K content. Six samples were unsuitable for livestock due to higher (Cl >30mgL- 1) Cl values. SSP rated 9 samples as “good”, 1 as “excellent”, 6 as “doubtful” and 9 as “permissible” for irrigation. With respect to RSC 21 samples were “suitable”, 3 were “marginal” and 1 was “unsuitable” for irrigation. Hardness classified 14 samples within “moderately hard”, 10 within “soft” and only one as “hard” limit for irrigation and 1 sample (No. 16) was unsuitable for livestock consumption. P, B, Cu and As concentration categorized all the samples suitable for irrigation, aquaculture, drinking and livestock consumption.DOI: http://dx.doi.org/10.3329/jesnr.v6i1.22053 J. Environ. Sci. & Natural Resources, 6(1): 131-140 2013

scholarly journals Cost-Effective Detection of Perfluoroalkyl Carboxylic Acids with Gas Chromatography: Optimization of Derivatization Approaches and Method Validation

2019 ◽  
Vol 17 (1) ◽  
pp. 100 ◽  
Author(s):  
Zhen Li ◽  
Hongwei Sun
Keyword(s):  
Gas Chromatography ◽  
Surface Water ◽  
Solid Phase Extraction ◽  
Carboxylic Acids ◽  
Water Samples ◽  
Solid Phase ◽  
Cost Effective ◽  
Phase Extraction ◽  
Surface Water Samples

The reliable quantification of perfluoroalkyl carboxylic acids (PFCAs) in environmental samples like surface water by using gas chromatography (GC) remains challenging because the polar PFCAs call for derivatization before injection and problems involving the integration of sample pretreatment and derivatization procedures. Here we proposed a cost-effective method for the GC based determination of C4–C12 PFCAs in surface water samples by integrating solid phase extraction and PFCAs anilide derivatization. First, we assessed the performance of different PFCAs derivatization methods, namely esterification and amidation. Esterification was unable to derivatize C4–C6 PFCAs. On the contrary, amidation procedures by using 2,4-difluoroaniline (DFA) and N,N′-dicyclohexylcarbodiimide (DCC) could successfully transform all the PFCA analogs to produce anilide derivatives, which could be easily detected by GC. Then the reaction conditions in the amidation approach were further optimized by using orthogonal design experiments. After optimizing the instrumental parameters of GC, the limits of detection (LOD) of this derivatization method were determined to be 1.14–6.32 μg L−1. Finally, in order to establish an intact method for the quantification of PFCAs in surface water samples, solid phase extraction (SPE) was used for extraction and cleanup, which was further integrated with the subsequent amidation process. The SPE-amidation-GC method was validated for application, with good accuracy and precision reflected by the PFCAs recoveries and derivatization of triplicates. The method reported here could provide a promising and cost-effective alternative for the simultaneous determination of C4–C12 PFCAs in environmental water samples.

scholarly journals Magnetic solid-phase extraction of caffeine from surface water samples with a micro–meso porous activated carbon/Fe3O4 nanocomposite prior to its determination by GC-MS

RSC Advances ◽  
2021 ◽  
Vol 11 (32) ◽  
pp. 19492-19499
Author(s):  
Natalia Manousi ◽  
Eleni A. Deliyanni ◽  
Erwin Rosenberg ◽  
George A. Zachariadis
Keyword(s):  
Activated Carbon ◽  
Surface Water ◽  
Water Samples ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Phase Extraction ◽  
Magnetic Solid ◽  
Surface Water Samples ◽  
Porous Activated Carbon ◽  
Solid Phase Material

A novel magnetic solid phase material based on a micro–meso porous activated carbon/Fe3O4 nanocomposite was used to extract caffeine from surface water samples. The method is efficient and rapid, and has minimum solvent consumption.

scholarly journals Determination of Hypoglycemic Agents in Surface Water Samples Using SPE-LC-MS/MS Method

2020 ◽  
Vol 71 (7) ◽  
pp. 337-346
Author(s):  
Vasile-Ion Iancu ◽  
Niculescu Marcela ◽  
Diana Puiu ◽  
Toma Galaon ◽  
Jana Petre ◽  
...  
Keyword(s):  
Surface Water ◽  
Water Samples ◽  
Emerging Contaminants ◽  
Solid Phase ◽  
Total Concentration ◽  
Hypoglycemic Agents ◽  
Number Of Patients ◽  
The World ◽  
Surface Water Samples

Antidiabetic compounds are a class of emerging contaminants in environment, for which there are no regulations in the world environmental legislation. These compounds are among the most widely used drugs in the world due to the large number of patients with diabetic conditions. The presence of these pollutants in the environment is insufficiently studied, so efficient analytical methods are needed to allow their detection at trace levels (ng/L). For the simultaneously quantification of the five antidiabetics (glyburide, metformin, glipizide, gliclazide, glimepiride) and one bio-degradation product (guanyl urea) in surface water samples a SPE-LC-MS/MS (solid phase extraction -liquid chromatography coupled with mass spectrometry detection) method was validated using real river water samples. The compounds were separated on C18 LC column in 9 minutes at 300C using a gradient of mobile phase of 0.1% formic acid and acetonitrile. Good performance parameters were obtained using the method: low limits of quantification (LOQs 0.1-2.4 ng/L), precision (repeatability 3.5-7.2% and reproducibility 6.5-12.7%) and determination coefficients (higher than 0.99). The most contaminated river was represented by Ialomita, which had a total concentration of antidiabetics of 112.1 ng/L in the downstream point, followed by the Siret and Dambovita rivers, which had a total concentration of antidiabetics of 66.3 ng/L and 57.3 ng/L, respectively, also in the downstream points.

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