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

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.

Download Full-text

Optimisation and validation of an automated solid phase extraction technique coupled on-line to enzyme-based biosensor detection for the determination of phenolic compounds in surface water samples

Chromatographia ◽

10.1007/bf02688027 ◽

1995 ◽

Vol 41 (5-6) ◽

pp. 207-215 ◽

Cited By ~ 19

Author(s):

E. Burestedt ◽

J. Emnéus ◽

L. Gorton ◽

G. Marko-Varga ◽

E. Domínguez ◽

...

Keyword(s):

Phenolic Compounds ◽

Surface Water ◽

Solid Phase Extraction ◽

Water Samples ◽

Solid Phase ◽

Phase Extraction ◽

On Line ◽

Surface Water Samples ◽

Automated Solid Phase Extraction

Download Full-text

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

International Journal of Environmental Research and Public Health ◽

10.3390/ijerph17010100 ◽

2019 ◽

Vol 17 (1) ◽

pp. 100 ◽

Cited By ~ 1

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.

Download Full-text

Determination of 4-tert-octylphenol in surface water samples of Jinan in China by solid phase extraction coupled with GC-MS

Journal of Environmental Sciences ◽

10.1016/s1001-0742(12)60209-5 ◽

2013 ◽

Vol 25 (8) ◽

pp. 1712-1717 ◽

Cited By ~ 7

Author(s):

Xueyu Yang ◽

Mingren Liu ◽

Zhongpeng Wang ◽

Qian Li ◽

Zhaoliang Zhang

Keyword(s):

Surface Water ◽

Solid Phase Extraction ◽

Water Samples ◽

Solid Phase ◽

Phase Extraction ◽

Surface Water Samples

Download Full-text

Optimisation and validation of an automated solid phase extraction technique coupled on-line to enzyme-based biosensor detection for the determination of phenolic compounds in surface water samples

Chromatographia ◽

10.1007/bf02267957 ◽

1995 ◽

Vol 41 (3-4) ◽

pp. 207-215 ◽

Cited By ~ 2

Author(s):

E. Burestedt ◽

J. Emnéus ◽

L. Gorton ◽

G. Marko-Varga ◽

E. Domínguez ◽

...

Keyword(s):

Phenolic Compounds ◽

Surface Water ◽

Solid Phase Extraction ◽

Water Samples ◽

Solid Phase ◽

Phase Extraction ◽

On Line ◽

Surface Water Samples ◽

Automated Solid Phase Extraction

Download Full-text

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

International Journal of Environmental Research and Public Health ◽

10.3390/ijerph17010134 ◽

2019 ◽

Vol 17 (1) ◽

pp. 134 ◽

Cited By ~ 1

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.

Download Full-text