Determination of Organochlorine, Organophosphorus and Pyrethroid Pesticide Residues in Water and Sediment Samples by High Performance Liquid Chromatography (HPLC) with UV/visible Detector

Author(s):  
Akan JC Sodipo OA
Author(s):  
Ling Wu ◽  
Qiurong He ◽  
Jing Zhang ◽  
Yongxin Li ◽  
Weiqing Yang ◽  
...  

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.


2021 ◽  
Vol 54 (2) ◽  
Author(s):  
Hassan Nabeel Ashraf ◽  
Noman Walayat ◽  
Muhammad Hamzah Saleem ◽  
Nadia Niaz ◽  
Abdul Hafeez ◽  
...  

2019 ◽  
Vol 11 (27) ◽  
pp. 3460-3466 ◽  
Author(s):  
Qilin Deng ◽  
Liping Sun ◽  
Tao Zhu

In this study, a new and green fluorinated chitosan (trifluoroethyl methacrylate-chitosan (TFEMA-CTS)) was synthesized, and the QuEChERS method was applied for the effective determination of four pesticide residues in apple samples by high performance liquid chromatography.


2020 ◽  
Vol 16 (1) ◽  
pp. 10
Author(s):  
Devi Wulandari ◽  
Gusrizal Gusrizal ◽  
Titin Anita Zaharah

<p>Telah dilakukan optimasi dan validasi metode penentuan asam glikolat dan asam laktat dalam krim menggunakan kromatografi cair kinerja tinggi. Pemisahan asam glikolat dan asam laktat dilakukan pada kolom fasa balik C-8menggunakan fasa gerak asam ortofosfat 0,1% dengan pH 3,5 dan detektor <em>UV-Visible</em>. Standar asam glikolat dan asam laktat dibuat dengan melarutkannya menggunakan asam ortofosfat 0,1% pH 3,5. Hasil eksperimen menunjukkan bahwa pada rentang konsentrasi 25 – 400 μg/mL, asam glikolat dan asam laktat memiliki kurva yang linear dengan koefisien korelasi masing-masing 0,9997 dan 0,9999. Uji presisi untuk larutan standar berkonsentrasi 100 µg/mL menghasilkan simpangan baku relatif sebesar 1,49% untuk asam glikolat dan 1,72% untuk asam laktat. Metode yang telah dioptimasi memberikan akurasi yang baik yang ditunjukkan oleh nilai perolehan kembali dari pengukuran tiga <em>spiked sample</em> dengan konsentrasi berbeda (50, 100, dan 150 μg/mL). Nilai perolehan kembali untuk masing-masing konsentrasi <em>spiked sample</em> adalah 97,12% ± 0,69; 98,76% ± 0,43; 100,80% ± 0,29 untuk asam glikolat dan 97,58% ± 0,39; 96,20% ± 0,68; 98,00% ± 0,38 untuk asam laktat. Batas deteksi dan batas kuantisasi untuk asam glikolat adalah 0,05 dan 0,17 μg/mL, sedangkan untuk asam laktat adalah 1,40 dan 4,67 μg/mL. Nilai kekasaran metode untuk asam glikolat pada hari pertama dan hari kedua adalah 1,43% dan 1,67%, sedangkan untuk asam laktat adalah 1,67% dan 1,25%. Metode yang telah dioptimasi dan divalidasi berpotensi untuk digunakan secara spesifik pada penentuan kadar asam glikolat dan asam laktat dalam krim.</p><p><strong>Optimization and Validation of Determination Methods of Glycolic Acid and Lactic Acid in Cream Using High-Performance Liquid Chromatography.</strong> A high-performance liquid chromatography analytical method for the determination of glycolic acid and lactic acid in creams has been optimized and validated. The separation was performed in a reverse phase C–8 column with a mobile phase of 0.1%, orthophosphoric acid at pH 3.5, and UV-Visible detector. The standard of glycolic acid and lactic acid was dissolved in 0.1% orthophosphoric acid at pH 3.5. The experimental results showed that in the concentration range of 25–400 μg/mL, glycolic acid and lactic acid showed a linear curve with a correlation coefficient of 0.9997 and 0.9999, respectively. The precision test for standard solutions containing 100 µg/mL resulted in a relative standard deviation of 1.49% for glycolic acid and 1.72% for lactic acid. The optimized method provided good accuracy indicated by the recovery of the measurement of three spiked samples in different concentrations (50, 100, and 150 μg/mL). The recovery for each concentration of the spiked sample was 97.12% ± 0.69; 98.76% ± 0.43; 100.80% ± 0.29 for glycolic acid and 97.58% ± 0.39; 96.20% ± 0.68; 98.00% ± 0.38 for lactic acid. The limit of detection and limit of quantization for glycolic acid was 0.05 and 0.17 μg/mL, and for lactic acid was 1.40 and 4.67 μg/mL. The ruggedness of the method for glycolic acid on the first day and second day was 1.43% and 1.67%, while for lactic acid, it was 1.67% and 1.25%. The method that has been optimized and validated shows the potential to be used specifically for the determination of glycolic acid and lactic acid in the cream.</p>


Nanomaterials ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 3319
Author(s):  
Nokwanda Hendricks ◽  
Olatunde Stephen Olatunji ◽  
Bhekumuzi Prince Gumbi

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.


Sign in / Sign up

Export Citation Format

Share Document