scholarly journals Simultaneous Determination of 2-Nitrophenol and 4-Nitrophenol in Pharmaceutical Industrial Wastewater by Electromembrane Extraction Coupled with HPLC-UV Analysis

2019 ◽  
Vol 25 (1) ◽  
pp. 57-64 ◽  
Author(s):  
Saeid Yaripour ◽  
Ali Mohammadi ◽  
Somayeh Mousavi ◽  
Isa Esfanjani ◽  
Naghmeh Arabzadeh ◽  
...  

Background: In the present study, an electromembrane extraction (EME) followed by a simple high performance liquid chromatography with ultraviolet detection (HPLC-UV) was developed and validated for simultaneous determination of 2-nitrophenol (2-NP) and 4-nitrophenol (4-NP) in pharmaceutical industrial wastewater sample. Main parameters of electromembrane extraction were evaluated and optimized. Methods: 1-octanol was immobilized in the pores of a polypropylene hollow fiber as supported liquid membrane. As a driving force, a 100 volt electrical voltage was applied to transfer the analytes from the sample solution (pH, 7.5) through the supported liquid membrane into an acceptor solution (pH, 12). Results: The best enrichment factors were obtained 36 and 72 for 2-NP and 4-NP, respectively after 15 minutes of extraction. The effect of carbon nanotube, as a solid nano-sorbent on EME efficiency, was also evaluated. The proposed method provided the linearity in the range of 10-1000 ng/mL for 2-NP (R2> 0.9997) and 4-NP (R2> 0.9999) with repeatability range (% RSD) between 2.6-10.3 % (n = 3). The limit of detection was 3 ng/mL and the limit of quantitation was 10 ng/mL. Conclusion: Finally, the method was applied for the determination of 2-NP and 4-NP in industrial wastewater samples with relative recoveries in the range between 67–76 %. EME improved the sensitivity of HPLC-UV for the determination of trace concentrations of these analytes.

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.


2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Dinh Quang Khieu ◽  
Mai Thi Thanh ◽  
Tran Vinh Thien ◽  
Nguyen Hai Phong ◽  
Duc Hoang Van ◽  
...  

Zeolite imidazole framework-8 (ZIF-8) was prepared by the hydrothermal process. The obtained ZIF-8 was a characteristic of X-ray-diffraction (XRD), transmission electron microscope (TEM), thermal gravity-differential thermal analysis (TG-DTA), and dynamic light scattering (DLS). The obtained ZIF-8 possessed large specific area and was highly dispersed. Its morphology consisted of nanospherical particles with 30–50 nm in diameter. Chemical stability of ZIF-8 in different conditions was studied. The ZIF-8 was used as an electrode modifier for the determination of trace levels of lead. The parameters including solvents and solution pH were investigated. The repeatability, reproducibility, accuracy, linear range, limit of detection, and limit of quantitation were also addressed. The results showed that ZIF-8 is a potential electrode modifier for differential pulse anodic stripping method to determine Pb(II) in aqueous solution.


Author(s):  
İsmail Murat Palabıyık ◽  
Aysegul Dogan ◽  
İncilay Süslü

Background: Hypertension is one of the most important health problems in the world and irbesartan and amlodipine are used in combination in various dosages for the treatment of high blood pressure. Objective: The aim of this study is to develop a fast, easy, sensitive, accurate, and precise square-wave voltammetry method for simultaneous determination of irbesartan and amlodipine besylate from pharmaceutical formulations at a hanging mercury drop electrode. Methods: In the applied method, since both active substances gave a peak at different potentials, no interference occurred between them. In optimization studies Britton-Robinson buffer of pH 8.0 was chosen, in which the most appropriate peak shape and maximum peak current were observed. At the same time, as a result of instrumental parameter optimization to obtain reproducible results, 6 mV for scan increment, 30 mV for pulse amplitude, and 50 Hz for frequency were found suitable. Results: As a result of the calibration studies of the optimized method, linear working ranges were determined as 1.00-13.08 µg mL-1 for irbesartan and 5.83-16.51 µg mL-1 for amlodipine besylate. Limit of detection and limit of quantitation values were respectively calculated as 0.63 and 1.00 µg mL-1 for irbesartan and 0.50 and 1.98 µg mL-1 for amlodipine besylate. The results of precision values (RSD) ranged from 0.67% to 2.31% for irbesartan and 0.65% to 1.49% for amlodipine besylate. Accuracy values were calculated as -0.15% to 1.63% for irbesartan and -0.07% to 3.78% for amlodipine besylate. The results obtained from the recovery studies ranged from 101.05% to 102.78% and from 98.88% to 102.20% for amlodipine besylate and irbesartan, respectively. Conclusion: After the validation studies of the developed method were carried out, it was successfully applied to pharmaceutical formulations containing these active substances.


1994 ◽  
Vol 77 (2) ◽  
pp. 344-350 ◽  
Author(s):  
Heidi S Rupp ◽  
Robert K Munns ◽  
Austin R Long ◽  
Steven M Plakas

Abstract A liquid chromatographic (LC) method was developed for the simultaneous determination of nitro-furazone (NFZ), nitrofurantoin (NFT), and furazolidone (FZD) in catfish muscle tissue. The drugs were extracted from the tissue with acetonitrile, and the lipids were removed from the extract with hexane. The acetonitrile extract was evaporated by rotary evaporation, and the resultant drug residues were dissolved with LC mobile phase. The mixture was sonicated, centrifuged, and filtered. The drugs were determined by using LC with a Cie reversed-phase (ODS Hypersil) column, a mobile phase of acetonitrile–1 % aqueous acetic acid (25 + 75), and a photodiode array ultraviolet detector at 375 nm. NFZ, NFT, and FZD were each determined in catfish tissue at 5 fortification levels (80, 40, 20,10, and 5 ng drug/g tissue). Average recoveries of each of the 3 drugs at each level ranged from 70.7 to 101.5%, and relative standard deviations ranged from 2.2 to 18.6%. The limit of detection of each drug was approximately 1 ng drug/g tissue, and the limit of quantitation was 5 ng drug/g tissue. In the second part of the study, the method was used to determine nitrofuran residues incurred in catfish tissue. Live channel catfish were intravascularly dosed (10 mg/kg body wt) with NFZ to generate drug-incurred fish muscle tissue. Incurred NFZ levels exceeded 400 ng drug/g tissue at 2 h after dosing but decreased rapidly to approximately 1 ng drug/g tissue by 8 h after dosing, as determined by this method.


2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Snehal J. More ◽  
Suparna S. Tandulwadkar ◽  
Ajinkya R. Nikam ◽  
Atul S. Rathore ◽  
L. Sathiyanarayanan ◽  
...  

A simple, precise, and accurate reversed-phase liquid chromatographic method has been developed for the simultaneous determination of paracetamol (PCM), chlorzoxazone (CHZ), and nimesulide (NIM) in pharmaceutical dosage form. The chromatographic separation was achieved on a Thermo Hypersil GOLD C18 column (250 × 4.6 mm i.d., 5 μm particle size). The mobile phase consisted of water : acetonitrile (55 : 45 v/v). The flow rate was set to 1.2 mL min−1 and UV detection was carried out at 275 nm. The retention time () for PCM, CHZ, and NIM was found to be 2.69 ± 0.02, 4.61 ± 0.01, and 9.55 ± 0.02 min, respectively. The validation of the proposed method was carried out for linearity, precision, robustness, limit of detection, limit of quantitation, specificity, and accuracy. The linear dynamic ranges were 32.5–65.0 μg mL−1 for PCM, 37.5–75.0 μg mL−1 for CHZ, and 10.0–20.0 μg mL−1 for NIM. The developed method can be used for routine quality control analysis of titled drugs in pharmaceutical dosage form.


2018 ◽  
Vol 69 (1) ◽  
pp. 27-30 ◽  
Author(s):  
Iuliana Paun ◽  
Vasile Ion Iancu ◽  
Liliana Cruceru ◽  
Marcela Niculescu ◽  
Florentina Laura Chiriac

A simple, reliable and accurate HPLC/CAD method was developed for the determination of anionic (sodium dioctyl sulfosuccinate and sodium 1-dodecane sulfonate), amphoteric (CHAPS (3-[(3-Cholamidopropyl) dimethylammonium]-1-propanesulfonate hydrate)) and cationic (benzethonium chloride) surfactants mixture from surface water samples. The chromatographic analysis was performed on an Acclaim Surfactant Plus (150 x 3.0 mm, 3 mm d.p.) column acquired from Thermo Scientific, kept at 300C. All experiments were performed in gradient elution conditions at a flow-rate of 0.6 mL/min. Mobile phase composition was a mixture of acetonitrile (A) and 0.1 M ammonium acetate solution acidified to pH 5 with acetic acid (B). The limit of detection (LD) were 20 mg/L for anionic surfactants and 30 mg/L for cationic and amphoteric surfactants. The calibration curves were linear between 15 mg/L � 110 mg/L, with R2 values above 0.992 for all surfactants. Solid phase extraction (SPE) using polymeric (Strata X) cartridges has been applied to extract and concentrate the target analytes from the synthetic samples. Surfactants recoveries after SPE procedure were situated between 91.5�94.6%. Intra-day and inter-day precision (RSD%) were situated between 4.0 � 7.7% and 7.5 � 11.7%, respectively. Limit of quantitation (LQ) was lower than 80 mg/L for anionic surfactants and 90 mg/L for cationic and 100 mg/L for amphoteric surfactants. The new sensitive and selective HPLC/CAD developed method allows simultaneous determination of anionic, amphoteric and cationic surfactants mixture from environmental samples (surface water).


2021 ◽  
Author(s):  
Ebrahim Nabatian ◽  
Mahdi Mousavi ◽  
Mostafa Pournamdari ◽  
Saeid Ahmadzadeh

Abstract A simple and precise analytical approach developed for single and simultaneous determination of resorcinol (RC) and hydroquinone (HQ) in pharmaceutical samples using carbon paste electrode (CPE) modified with 1-Ethyl-3-methylimidazolium tetrafluoroborate as ionic liquid and ZnFe2O4 nanoparticle. A significant enhancement in the peak current and sensitivity of the proposed sensor observed by using modifiers in the composition of working electrode compared to bare CPE which is in accordance with the results obtained from electrochemical impedance spectroscopy investigations. Electrochemical investigations revealed a well-defined irreversible oxidation peak for RC over a wide concentration range from 3.0 µM to 500 µM in 0.1 M phosphate buffer solution (pH 6.0) with the linear regression equations of Ip (µA) = 0.0276 CRC (µM) + 0.5508 (R2 = 0.997). The limit of detection and quantification for RC analysis were found to be 1.46 µM and 4.88 µM, respectively. However, the obtained SW voltammograms for simultaneous determination of RC and HQ exhibited a desirable peak separation of about 360 mV potential difference and a satisfactory linear response over the range of 50-700 µM and 5-350 µM with the favorable correlation coefficient of 0.991 and 0.995, respectively. The diffusion coefficient (D) of RC and the electron transfer coefficient (α) at the surface of ZnFe2O4/NPs/IL/CPE estimated to be 2.83×10−4 cm s−1 and 0.76. The proposed sensor as a promising and low-cost method successfully applied for determination of RC in commercial pharmaceutical formulations such as the resorcinol cream of 2% O/W emulsion available on the market with the recovery of 98.47±0.04.


Author(s):  
Narendra M. Gowekar ◽  
Shailesh J Wadher

  Objective: A simple, specific, accurate, and precise method, namely, reverse phase high-performance liquid chromatography was to develop for simultaneous estimation of Lidocaine (LDC) and prilocaine (PLC) in a topical local anesthetic cream.Method: The mixture of PLC and LDC was separated on Hi Q Sil C18 HS column, (250 mm × 4.6 mm, 5 μm), column temperature ambient and flow rate 1.2 mL/minutes. The mobile phase was acetonitrile: 0.01 M diethylamine solution (pH adjusts to 6.8 with orthophosphoric acid) (60:40) with detection at 225 nm.Results: The retention time was found to be 6.075±0.12 minutes for PLC and 8.642±0.15 minutes for LDC, respectively. Linearity was observed in the concentration range of 1-6 μg/mL for both LDC and PLC, respectively. The method was validated according to International Conference on Harmonization guideline and values of linearity, precision, robustness, limit of detection, limit of quantitation, selectivity, and recovery were found to be in good accordance with the prescribed value.Conclusion: The proposed method can be useful in the quality control of LDC and PLC in their topical formulation.


Sign in / Sign up

Export Citation Format

Share Document