scholarly journals Simultaneous Determination of Four Nonsteroidal Anti-Inflammatory Drugs and Three Estrogen Steroid Hormones in Wastewater Samples by Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplet and HPLC

2020 ◽  
Vol 103 (2) ◽  
pp. 392-398 ◽  
Author(s):  
Mihail Simion Beldean-Galea ◽  
Romain Klein ◽  
Maria-Virginia Coman

Abstract Background: Nonsteroidal anti-inflammatory drugs (NSAIDs) and estrogen steroid hormones (estrogens) are pharmaceuticals intensively studied in environmental analysis due to their toxic effect on animal and human beings. Objective: Development of a simple, fast, and sensitive extraction method for the simultaneously analysis of four NSAIDs (ketoprofen, naproxen, ibuprofen, and diclofenac) and three estrogens (17ß-estradiol, 17α-ethynylestradiol, and estriol) from wastewater samples. Method: Dispersive liquid–liquid microextraction based on solidification of floating organic droplet followed by HPLC analysis with UV detection was developed. The influence of the main extraction parameters, e.g., the volume of extraction solvent and of disperser, the pH, and the ionic strength of sample were evaluated. Results: Good resolutions between the selected drugs were obtained using a reverse-phase column and a mobile phase of acetonitrile and water. This method provides good linearity (r > 0.999) in a concentration range of 1–100 µg/mL, good intra- and inter-day precision (RSD <7%) and low LOQs. The obtained enrichment factors were ranged between 162 and 180 for NSAIDs and between 118 and 185 for estrogens. The relative recoveries were situated >80% for all analysed drugs, except estriol (59%) both in synthetic and real wastewater samples. Conclusions: The developed method has been successfully applied for the analysis of the selected drugs in wastewater samples collected from the influent of a wastewater treatment plant. Highlights: Four NSAIDs and three estrogens from wastewater samples were simultaneously extracted and analysed using only 10 mL of sample and 50 μL of extraction solvent.

2014 ◽  
Vol 881-883 ◽  
pp. 631-634 ◽  
Author(s):  
Jian Qi Sun ◽  
Ming Tang ◽  
Jun Dai

A simple and reliable method combining dispersive liquid-liquid microextracion (DLLME) with gas chromatography (GC) using flame ionization detection (FID) was developed for the simultaneous determination of aniline (AL),o-toluidine (o-TLD),N,N-dimethylaniline (N,N-DAL),p-chloroaniline (p-CAL), andp-nitroaniline (p-NAL) in wastewater. For this purpose, dispersive liquid-liquid microextraction (DLLME) was applied as a sample preparation technique. The DLLME conditions such as the types and volume of extraction solvent, the types and volume of the disperser solvent, pH value and salt addition were studied and optimized. The method was linear in the ranges from 2.2×10-3to 100.0 μg·mL-1for aforementioned aromatic amines withR2≥ 0.9968. The DLLME procedure allowed efficient recovery of the investigated aromatic amines ranging between 82 % and 92 % with a relative standard deviation (RSD) ≤ 3.4 for actual wastewater samples spiked with 5, 10 and 20 μg·mL-1of aromatic amines, respectively. These results showed the potential of this technique for aromatic amines monitoring in wastewater samples. Furthermore, the investigated methods are simple, reproducible, and inexpensive.


Water ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1581 ◽  
Author(s):  
Hryniewicka ◽  
Starczewska ◽  
Gołębiewska

Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) was applied to isolate budesonide (BUD) and sulfasalazine (SULF) from aqueous samples. The effects of different parameters on the efficiency on the extraction such as type of extrahent and dispersive solvent, ionic strength, pH of sample, and centrifugation time were investigated. Moreover, the influence of foreign substances on a studied process was tested. The calibration curves were recorded. The linearity ranges for BUD and SULF were 0.022–8.611 µg mL−1 and 0.020–7.968 µg mL−1 with the limit of detection (LOD) 0.011 µg mL−1 and 0.012 µg mL−1, respectively. The enrichment factors (EF) for two analytes were high: for BUD it was 145.7 and for SULF, 119.5. The elaborated procedure was applied for HPLC-UV determination of these analytes in water and wastewater samples.


2014 ◽  
Vol 6 (18) ◽  
pp. 7294-7304 ◽  
Author(s):  
Yu Ji ◽  
Zhenxia Du ◽  
Haojie Zhang ◽  
Yun Zhang

A novel rapid analytical method for the determination of four non-steroidal anti-inflammatory drugs (NSAIDs) – nabumetone, ibuprofen, naproxen and diclofenac – in tap water and drinks is presented.


2014 ◽  
Vol 881-883 ◽  
pp. 627-630 ◽  
Author(s):  
Jian Qi Sun ◽  
Fang Zeng ◽  
Xiao Feng Liu

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of acrylates (methyl acrylate (MA), methyl methacrylate (MMA), butyl acrylate (BA)) in wastewater. For this purpose, dispersive liquid-liquid microextraction (DLLME) was applied as a sample preparation technique. The DLLME conditions such as the types and volume of extraction solvent, the types and volume of the disperser solvent, pH value and salt addition were studied and optimized. The method was linear in the ranges from 4.3×10-4 to 200.0 μg·mL-1 for abovementioned acrylates with R2≥ 0.9992. The DLLME procedure allowed efficient recovery of the investigated acrylates ranging between 81 % and 109 % with a relative standard deviation (RSD) ≤ 9.1 for the blank samples spiked with 10, 50 and 100 μg·mL-1 of acrylates, respectively. These results showed the potential of this technique for acrylates monitoring in wastewater samples. Furthermore, the investigated methods are simple, reproducible, and inexpensive.


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