scholarly journals Quantification and Ecological Risk Assessment of Colloidal Fullerenes Nanoparticles in Sediments by Ultrasonic-Assisted Pressurized Liquid Extraction and High Performance Liquid Chromatography

Nanomaterials ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 3319
Author(s):  
Nokwanda Hendricks ◽  
Olatunde Stephen Olatunji ◽  
Bhekumuzi Prince Gumbi
Keyword(s):  
Risk Assessment ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ecological Risk ◽  
High Performance ◽  
Liquid Extraction ◽  
Environmental Concentration ◽  
Sediment Samples ◽  
Ultrasonic Assisted

Fullerenes engineered nanomaterials are regarded as emerging environmental contaminants. This is as their widespread application in many consumer products, as well as natural release, increases their environmental concentration. In this work, an ultrasonic-assisted pressurized liquid extraction (UAPLE) method followed by high performance liquid chromatography with ultraviolet-visible detector (HPLC-UV-vis) was developed for extraction and determination of fullerene in sediments. The method was validated and found to be suitable for environmental risk assessment. Thereafter, the method was used for the determination of fullerene (C61-PCBM) in sediment samples collected from Umgeni River, South Africa. The current method allows for adequate sensitivity within the linear range of 0.01–4 µg g−1, method limit detection of 0.0094 µg g−1 and recoveries ranged between 67–84%. All the parameters were determined from fortified sediments samples. The measured environmental concentration (MEC) of fullerene in the sediment samples ranged from not detected to 30.55 µg g−1. To the best of our knowledge, this is the first report on the occurrence and ecological risk assessment of carbonaceous fullerene nanoparticles in African sediments and biosolids.

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.

scholarly journals Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

2019 ◽  
Vol 6 (8) ◽  
pp. 190952 ◽  
Author(s):  
Nur Hidayah Sazali ◽  
Anas Alshishani ◽  
Bahruddin Saad ◽  
Ker Yin Chew ◽  
Moi Me Chong ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Vitamin D3 ◽  
High Performance ◽  
Liquid Extraction ◽  
Sample Treatment ◽  
Salting Out ◽  
Milk Samples ◽  
Liquid Liquid Extraction

In this study, salting-out assisted liquid–liquid extraction (SALLE) as a simple and efficient extraction technique followed by high-performance liquid chromatography (HPLC) was employed for the determination of vitamin D3 in milk samples. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. Under the optimum conditions, acetonitrile and ammonium sulfate were used as the extraction solvent and salting-out agent, respectively. The vitamin D3 extract was separated using Hypersil ODS (250x i.d 4.6 mm, 5 µm) HPLC column that was coupled with diode array detector. Vitamin D2 was used as internal standard (IS) to offset any variations in chromatographic conditions. The vitamin D3 and the IS were eluted in 18 min. Good linearity ( r 2 > 0.99) was obtained within the range of 25–600 ng g −1 with the limit of detection of 15 ng g −1 and limit of quantification of 25 ng g −1 . The validated method was applied for the determination of vitamin D3 in milk samples. The recoveries for spiked samples were from 94.4 to 113.5%.

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