Development of an analytical method for the simultaneous determination of the 17 EU Watch List compounds in surface waters: a Spanish case study

2018 ◽  
Vol 15 (8) ◽  
pp. 493
Author(s):  
José Luis Malvar ◽  
Concepción Abril ◽  
Julia Martín ◽  
Juan Luis Santos ◽  
Irene Aparicio ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Organic Pollutants ◽  
Surface Waters ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Anthropogenic Activities ◽  
Watch List ◽  
The Eu

Environmental contextIn 2015, the European Union issued a Watch List of organic pollutants resulting from anthropogenic activities. A major obstacle to controlling these pollutants in the environment is the difficulty of their simultaneous measurement at low concentrations. We developed an analytical method for the simultaneous determination in surface water of the 17 pollutants included in the EU Watch List. AbstractA multi-class method was developed for the simultaneous determination of the 17 organic pollutants included in the EU Decision 2015/495 regarding surface waters. The target analytes were three estrogens, four pharmaceuticals, a food additive, a solar filter and eight pesticides. The target compounds were extracted through solid-phase extraction with Oasis HLB cartridges. Determination was carried out by high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). All compounds were satisfactorily determined in one single injection, with a chromatographic run time of only 20min. The limit of detection (LOD) of the proposed method was in the range of 0.08–13ngL−1. For most of the target compounds, except for 17α-ethinylestradiol, 17β-estradiol and estrone, the LOD values were equal or below those required by the EU Decision 2015/495. Accuracy was in the range of 69–120%, whereas inter-day variability was below 20% in all cases. The validated method was applied to assess the presence of these compounds in Mediterranean surface waters. Samples were collected from 18 sampling sites located in the south of Spain. Up to 14 compounds were detected, among them, the pharmaceutical compounds were the pollutants most frequently detected at concentration levels up to 1158ngL−1 (diclofenac).

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

scholarly journals Determination of Pharmaceutical Residues by UPLC-MS/MS Method: Validation and Application on Surface Water and Hospital Wastewater

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Bui Van Hoi ◽  
Cam-Tu Vu ◽  
Lan-Anh Phung-Thi ◽  
Thao Thi Nguyen ◽  
Phuong Thanh Nguyen ◽  
...  
Keyword(s):  
Surface Water ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Hospital Wastewater ◽  
Esi Ms ◽  
Pharmaceutical Residues ◽  
Detection Frequency

In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005–0.015 µg L−1 and 0.014–0.123 µg L−1, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.

Simultaneous Determination of Anionic, Amphoteric and Cationic Surfactants Mixtures in Surface Water

2018 ◽  
Vol 69 (1) ◽  
pp. 27-30 ◽  
Author(s):  
Iuliana Paun ◽  
Vasile Ion Iancu ◽  
Liliana Cruceru ◽  
Marcela Niculescu ◽  
Florentina Laura Chiriac
Keyword(s):  
Surface Water ◽  
Simultaneous Determination ◽  
Cationic Surfactants ◽  
Anionic Surfactants ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Acetate Solution ◽  
Limit Of Quantitation ◽  
Amphoteric Surfactants

A simple, reliable and accurate HPLC/CAD method was developed for the determination of anionic (sodium dioctyl sulfosuccinate and sodium 1-dodecane sulfonate), amphoteric (CHAPS (3-[(3-Cholamidopropyl) dimethylammonium]-1-propanesulfonate hydrate)) and cationic (benzethonium chloride) surfactants mixture from surface water samples. The chromatographic analysis was performed on an Acclaim Surfactant Plus (150 x 3.0 mm, 3 mm d.p.) column acquired from Thermo Scientific, kept at 300C. All experiments were performed in gradient elution conditions at a flow-rate of 0.6 mL/min. Mobile phase composition was a mixture of acetonitrile (A) and 0.1 M ammonium acetate solution acidified to pH 5 with acetic acid (B). The limit of detection (LD) were 20 mg/L for anionic surfactants and 30 mg/L for cationic and amphoteric surfactants. The calibration curves were linear between 15 mg/L � 110 mg/L, with R2 values above 0.992 for all surfactants. Solid phase extraction (SPE) using polymeric (Strata X) cartridges has been applied to extract and concentrate the target analytes from the synthetic samples. Surfactants recoveries after SPE procedure were situated between 91.5�94.6%. Intra-day and inter-day precision (RSD%) were situated between 4.0 � 7.7% and 7.5 � 11.7%, respectively. Limit of quantitation (LQ) was lower than 80 mg/L for anionic surfactants and 90 mg/L for cationic and 100 mg/L for amphoteric surfactants. The new sensitive and selective HPLC/CAD developed method allows simultaneous determination of anionic, amphoteric and cationic surfactants mixture from environmental samples (surface water).

scholarly journals Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Alternaria Toxins in Grapes

Toxins ◽  
2019 ◽  
Vol 11 (2) ◽  
pp. 87 ◽  
Author(s):  
Wenbo Guo ◽  
Kai Fan ◽  
Dongxia Nie ◽  
Jiajia Meng ◽  
Qingwen Huang ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Safe Procedure ◽  
Alternariol Monomethyl Ether ◽  
Limit Of Quantification ◽  
Alternaria Toxins ◽  
Relative Standard

A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six Alternaria toxins. After validation by determining the linearity (R2 > 0.99), recovery (77.8–101.6%), sensitivity (limit of detection in the range of 0.03–0.21 μg kg−1, and limit of quantification in the range of 0.09–0.48 μg kg−1), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of Alternaria toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with Alternaria toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10–1.64 μg kg−1, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the Alternaria toxins contamination in grapes in China.

Improved derivatization protocol for simultaneous determination of alkylphenol ethoxylates and brominated flame retardants followed by gas chromatography-mass spectrometry analyses

2014 ◽  
Vol 69 (12) ◽  
pp. 2389-2396 ◽  
Author(s):  
T. B. Chokwe ◽  
J. O. Okonkwo ◽  
L. L. Sibali ◽  
E. J. Ncube
Keyword(s):  
Simultaneous Determination ◽  
Environmental Samples ◽  
Flame Retardants ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Brominated Flame Retardants ◽  
Gas Chromatography Mass Spectrometry ◽  
Alkylphenol Ethoxylates ◽  
Limit Of Quantification

An improved derivatization protocol for the simultaneous determination of alkylphenol ethoxylates and brominated flame retardants with heptafluorobutyric anhydride under triethylamine amine base was investigated. The derivatization reaction was completed in 30 min at 50 °C using hexane as solvent. Under these conditions, it was observed that alkylphenol ethoxylates and tetrabromobisphenol A were derivatized successfully in the presence of hexabromocyclododecane, lower congeners of polybrominated biphenyls and polybrominated diphenyl ethers. The improved protocol was applied to the recover of the analytes of interest from a simulated water sample after solid phase extraction. The recoveries achieved were above 60%. The limit of detection and limit of quantification ranged from 0.01–0.20 and 0.05–0.66 μg L−1, respectively. The improved derivatization procedure was also successfully applied to determine trace amounts of these compounds in environmental water samples. The concentrations of the targeted analytes from the environmental samples were determined from limit of quantification. The levels of the targeted compounds in the environmental samples ranged from nd-7.63 ±2.83 μg L−1.

Simultaneous Determination of Nitrofurazone and Furazolidone in Shrimp (Penaeus vannamei) Muscle Tissue by Liquid Chromatography with UV Detection

1993 ◽  
Vol 76 (6) ◽  
pp. 1235-1239 ◽  
Author(s):  
Heidi S Rupp ◽  
Robert K Munns ◽  
Austin R Long
Keyword(s):  
Simultaneous Determination ◽  
Muscle Tissue ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Column ◽  
Aqueous Acetic Acid ◽  
Uv Detector ◽  
Relative Standard

Abstract A liquid chromatographic (LC) method was developed for the simultaneous determination of nitrofurazone (NFZ) and furazolidone (FZD) in shrimp muscle tissue. The drugs are extracted from the tissue with acetonitrile, and the lipids and lipophilic pigments are removed from the extract with hexane. The remaining acetonitrile extract is evaporated by rotary evaporation, and the resultant residues are dissolved with LC-grade water, applied to a preconditioned C18 solid-phase extraction column, and eluted with acetonitrile. The acetonitrile eluant is then dried under nitrogen, and the resultant drug residues are dissolved with mobile phase and filtered. The drugs are determined by LC by using a C18 reversed-phase (octyldecylsilyl Hypersil) column, a mobile phase of acetonitrile- 1% aqueous acetic acid (25 + 75, v/v), and a photodiode array UV detector at 375 nm. NFZ and FZD were determined in shrimp tissue at each of 5 spiking levels (64,32,16, 8, and 4 ng drug/g tissue). Absolute recoveries ranged from 70.6 to 78.4%, and relative standard deviations ranged from 4.0 to 13.6%. The limit of detection of pure standard of each drug was approximately the equivalent of 1 ng drug/g tissue, and the limit of determination in a sample was 4 ng drug/g tissue.

scholarly journals A simple analytical method for the simultaneous determination of multiple organic pollutants in sediment samples

MethodsX ◽  
2018 ◽  
Vol 5 ◽  
pp. 1089-1094 ◽  
Author(s):  
Xiangying Zeng ◽  
Qiongpu Hu ◽  
Lixiong He ◽  
Zhiyang Liu ◽  
Shutao Gao ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Organic Pollutants ◽  
Analytical Method ◽  
Sediment Samples ◽  
Simple Analytical Method

Reverse-phase HPLC method for the simultaneous analysis of triclosan and triclocarban in surface waters

2010 ◽  
Vol 10 (2) ◽  
pp. 173-180 ◽  
Author(s):  
Irena Baranowska ◽  
Sylwia Magiera ◽  
Katarzyna Bortniczuk
Keyword(s):  
Simultaneous Determination ◽  
Surface Waters ◽  
Extraction Method ◽  
Mobile Phase ◽  
Solid Phase ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Reverse Phase Hplc ◽  
Reverse Phase

A validated reverse-phase HPLC-DAD for the simultaneous determination of triclosan and triclocarban in surface water has been developed, because this method has not been used for determination of these disinfectant agents so far. An isocratic elution was achieved using a Develosil RP Aqueous AR-5 RP-30 column with a flow rate of 1.0 mL min−1. The mobile phase consisted of mixed methanol and water in raito of 90:10, v/v. DAD detector was used to monitor the analytes at 280 nm for triclosan and 265 nm for triclocarban. The time of analysis was 10 min and the retention time for triclosan and triclocarban was 5.81 min and 8.13 min, respectively. The solid phase extraction method was proposed for the preconcentration step. The extraction efficiencies were approximately 97% for triclosan and 87% for triclocarban. The linearity range for triclosan and triclocarban after pre-concentration were between 0.5–20 μg mL−1 and 0.3–20 μg mL−1, respectively. The LOD and LOQ of triclosan and triclocarban in real samples were 0.04 ng mL−1 and 0.11 ng mL−1, 0.17 ng mL−1 and 0.50 ng mL−1, respectively. The method has been sensitive and can be successfully applied to the fast and simultaneous determination of triclosan and triclocarban in surface waters.

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