scholarly journals A Fast Ultrasound-assisted Extraction Sample Preparation for Multi-elemental Determination of Contaminants in Pharmaceutical Ingredients by ICP-MS

2017 ◽  
Vol 38 (6) ◽  
pp. 165-173 ◽  
Author(s):  
Giovanna de Fatima Moreno Aguiar ◽  
Bruno Lemos Batista ◽  
Eloísa Silva de Paula ◽  
Andres Dobal Campíglia ◽  
Fernando Barbosa Jr.
Keyword(s):  
Sample Preparation ◽  
Ultrasound Assisted Extraction ◽  
Pharmaceutical Ingredients ◽  
Assisted Extraction ◽  
Icp Ms ◽  
Elemental Determination ◽  
Ultrasound Assisted

QuEChERS with ultrasound-assisted extraction combined with high-performance liquid chromatography for the determination of 16 polycyclic aromatic hydrocarbons in sediment

2021 ◽  
Author(s):  
Ling Wu ◽  
Qiurong He ◽  
Jing Zhang ◽  
Yongxin Li ◽  
Weiqing Yang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Aromatic Hydrocarbons ◽  
High Performance ◽  
Ultrasound Assisted Extraction ◽  
Sediment Samples ◽  
Assisted Extraction ◽  
Polycyclic Aromatic ◽  
Ultrasound Assisted

Abstract Background Polycyclic aromatic hydrocarbons (PAHs) have attracted worldwide attention due to their carcinogenic, teratogenic and mutagenic effects, environmental persistence and bioaccumulation characteristics. Therefore, the sensitive, reliable and rapid detection of PAHs in sediment is of great importance. Objective To develop a high-performance liquid chromatography (HPLC) with fluorescence and ultraviolet detection after QuEChERS treatment for simultaneous determination of 16 U.S. Environmental Protection Agency priority PAHs in sediment samples. Methods The samples were ultrasonically extracted with acetone and then the supernatant was purified with a modified QuEChERS method. After centrifugation, the supernatant was injected into the HPLC system for analysis. The separation was accomplished on a ZORBAX Eclipse PAH column (150 × 4.6 mm, 3.5 μm) and the column temperature was set at 30 °C. The flow rate of the mobile phase consisting of water and acetonitrile in gradient elution mode was fixed at 0.9 mL/min. Detection was conducted on an ultraviolet detector and a fluorescence detector simultaneously. The qualitative analysis was based on retention time and the quantification was based on standard curves. Results Under the optimal conditions, this method showed good linearities in the range of 10–200 μg/L with correlation coefficients greater than 0.9993. The method had the limits of detection (LODs) ranging from 0.00108 to 0.314 ng/g. The mean recoveries ranged from 78.4 to 117% with the intra-day and inter-day relative standard deviations (RSDs) of 0.592–10.7 and 1.01–13.0%, respectively. The proposed method was successfully applied to the detection of 16 PAHs in sediment samples collected from the Funan River in Chengdu, China with the total contents of 431 to 2143 ng/g·dw. Conclusions The established method is simple, rapid, environment-friendly and cost- effective. It can be applied to the analysis of 16 PAHs in sediment samples. Highlights A method of QuEChERS with ultrasound-assisted extraction combined with HPLC has been established for the analysis of 16 PAHs in sediment samples and the proposed method has been successfully applied to the analysis PAHs in real sediment samples.

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