Occurrence of Novel Perfluoroalkyl Ether Carboxylic Acids in River Water and Human Urine Quantified by a Simple Liquid–Liquid Microextraction Approach Coupled with LC–MS/MS

Author(s):  
Jingzhi Yao ◽  
Yitao Pan ◽  
Yu Huan ◽  
Jiayin Dai
2021 ◽  
Vol 13 (35) ◽  
pp. 3978-3986
Author(s):  
Corinna Fischer ◽  
Thomas Göen

A method is presented for the extraction of the UV stabilizer UV-327 and its metabolites from urine with acetonitrile (disperser solvent) and chloroform (extraction solvent), followed by instrumental analysis of the trimethylsilylated analytes.


2019 ◽  
Vol 102 (3) ◽  
pp. 942-951 ◽  
Author(s):  
Danni Yang ◽  
Yi Yang ◽  
Yongxin Li ◽  
Shuo Yin ◽  
Yaling Chen ◽  
...  

Abstract Background: Consistent toxicological evidence indicate that phthalates can cause adverse effects on human health. The concern over phthalate pollution and exposure has been emphasized in recent years. Therefore, the sensitive, reliable, and rapid detection of phthalates in water is of great importance. Objective: In this study, dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) combined with HPLC-UV detection was established and applied in the preconcentration and detection of 15 phthalates in drinking and river water samples. Methods: A mixture of acetonitrile (dispersant) and 1-dodecanol (extractant) was injected into water samples, which had been added with sodium chloride. The cloudy solution was formed by hand-shaking. After centrifugation, the sample solution was cooled in a refrigerator, and the solidified organic droplet was collected. It melted at room temperature and was injected into the HPLC system for analysis. The quantification was based on the working curves. Results: Under optimum conditions, this method showed good linearity in the range of 0.1–100 or 0.5–100 μg/L with correlation coefficients greater than 0.999. The method had the LODs ranging from 0.013 to 0.16 μg/L with the enrichment factors of 102–218. The recoveries of the method ranged from 86.8 to 119% with RSDs less than 12.6%. The interday and intraday RSDs were 6.35–13.5% and 3.00–13.7%, respectively. The established method has been successfully applied to the analysis of phthalates in drinking and river waters. Conclusions: The established method is rapid, sensitive, cost-effective, and environmentally friendly. It can be applied to the analysis of 15 phthalates in drinking and river water samples. Highlights: A method of DLLME-SFO combined with HPLC-UV detection has been established for the analysis of 15 phthalates in drinking and river water samples. The established method was rapid, sensitive, accurate, cost-effective, and environmentally friendly. The established method was successfully applied to the analysis of 15 phthalates in bottled, tap, and river water samples.


2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Walaa El-Alfy ◽  
Omnia A. Ismaiel ◽  
Magda Y. El-Mammli ◽  
Abdalla Shalaby

A simple RP-HPLC-PDA method for determination of atenolol (ATN) and trimetazidine (TMZ) in human urine and tablets has been developed. Analytes were separated on a Caltrex BI column (125× 4.0 mm, 5 μm) with 25mM potassium dihydrogen phosphate pH 3.3, methanol, and acetonitrile mobile phases. The PDA detector was operated at 210 nm for TMZ and 225 nm for ATN and the flow rate was 1.0 mL/ min. Linearity was obtained over a concentration range of (1.0-100 μg/mL) for both analytes in standard solutions and the method was successfully applied for determination of target analytes in their pharmaceutical tablets. Excellent linearity was also obtained over concentration ranges of (0.25-25 μg/mL) and (0.5-25 μg/mL) in human urine for TMZ and ATN, respectively. A simple liquid-liquid extraction was applied for urine sample clean-up and a gradient method was used for chromatographic separation. The lower limit of quantitation (LOQ) was 0.99 and 0.60 μg/mL for ATN and TMZ, respectively. The limit of detection (LOD) was 0.30 and 0.18 μg/mL for ATN and TMZ, respectively. Inter- and intraday precision and accuracy for ATN were within ±1.89% in pure form and within ±2.85% in urine samples. Inter- and intraday precision and accuracy for TMZ were within ± 3.99% in pure form and within ± 3.19% in urine samples.


Sign in / Sign up

Export Citation Format

Share Document