A hplc-uv method for deteermination of three pesticides in water

HPLC method is developed and validated for determination of three pesticides (abamectin, imidacloprid, and -cyfluthrin) in water. These pesticides are used widely in agriculture for crops protection, and may be leached to the groundwater. Reversed-phase method with C18 column (5 μm, 250mm × 4.6 mm inner diameter) using a mobile phase consisting of acetonitrile/water (v:v = 4:1) at a flow rate of 1.5 mL/min and UV detection at 220 nm was used. This method is validated according to new methods which include accuracy, precision, linearity and range, limit of detection and limit of quantitation. The current method exhibits good linearity over the range of 1-1000 ppb for abamectin, 0.5-1000 ppb for imidacloprid, and 0.4-1000 ppb for ß-cyfluthrin with r2 greater than 0.990. The percentage recovery of the method at three concentration levels (5, 100, and 1000 ppb) is within 97.6 to 101.5% for the three pesticides. Relative standard deviation of the area of six replicate injections of each pesticide at three concentration levels (5.0, 100.0, and 1000.0 ppb) was found to be less than 1% which reflect the precision of the method. Limit of quantitation of the three pesticides using this method is low (1.0, 0.5, and 0.4 ppb) for abamectin, imidacloprid, and -cyfluthrin, respectively which enables the determination of these three pesticides in water at low concentration levels

Development and Validation of HPLC-UV Method for Determination of Bovine Serum Albumin and Myoglobin Proteins

A simple HPLC with UV detection method is developed and validated for determination of Bovine Serum Albumin and Myoglobin proteins in a standard solution of the two protein as well as in a plasma spiked with theses two proteins. Separation was achieved on a reversed-phase C18, 5.0 μm, 150mm × 4.6 mm inner diameter column using a mobile phase consisting of solution A (900 mL of water, 100 mL Acetonitrile, 10 mL Trifluroacetic acid) and solution B (900 mL of acetonitrile, 100 mL water, 10 mL Trifluroacetic acid) with gradient elution of 5 to 50% of solution B in 15 minutes. This new method is validated in accordance with requirements for new methods, which include accuracy, precision, selectivity, linearity and range, robustness, limit of detection and limit of quantitation. The method demonstrates good linearity over the range of 1-1000 ppm for the two proteins with r2 greater than 0.998. The percentage recovery of the method is within 97.9 to 102.0% for the two proteins. Precision of this method reflected by relative standard deviation of the area of six replicate injections of each protein at five concentration levels (1.0, 100.0, 300.0, 500, and 1000.0 ppm) was found to be less than 2%. Limit of quantitation of the two proteins is low which enables the determination of these proteins at low concentration

Development and Validation of a Simple Reversed‑Phase HPLC‑UV Method for Determination of Malondialdehyde in Olive Oil

A simple, precise, accurate and selective method was developed and validated for determination of malondialdehyde (MDA) in olive oil. Separation was achieved on a reversed-phase C8 column using a mobile phase consisting of methanol/0.8 % phosphoric acid (10:90, v/v), at a flow rate of 1.0 ml/min and UV detection at 220 nm. This method was validated according to the requirements for new methods, which include accuracy, precision, selectivity, robustness, a limit of detection, limit of quantitation (LOQ), linearity and range. The current method demonstrated good linearity over the range of 0.5–1000 ppm of MDA with r2 greater than 0.999. The recovery of MDA in olive oil ranged from 97.1 to 99.1 %. The method was selective where MDA was distinctly separated from other compounds of the oil with good resolution. The method was also precise where the RSD of the peak areas of replicate injections of MDA standard solution were less than 1 %. The degree of reproducibility of the results obtained as a result of small deliberate variations in the method parameters and by changing the analytical operators proved that the method is robust and rugged. The low LOQ of MDA (0.5 ppm) using this method enables quantitation of MDA at low concentration

Berberine, a popular dietary supplement for human and animal health: Quantitative research literature analysis – a review

Berberine is an alkaloid with a wide range of reported beneficial health effects. The current work provides an extensive literature analysis on berberine. Bibliometric data were identified by means of the search string TOPIC=(“berberin*” OR “umbellatine*”), which yielded 5,547 publications indexed in the Web of Science Core Collection electronic database. The VOSviewer software generated bubble maps to visualize semantic terms with citation results. The ratio of original articles to reviews was 13.6:1. The literature has been growing more quickly since the 2010s. Major contributing countries were China, the United States, India, Japan, and South Korea. Most of the publications appeared in journals specialized in pharmacology pharmacy, biochemistry molecular biology, chemistry, and plant science. Some of the frequently mentioned chemicals/chemical classes were alkaloid, palmatine, jatrorrhizine, coptisine, isoquinoline, and sanguinarine. The prevalent medical conditions under investigation included Alzheimer’s disease, cancer, diabetes, and obesity

Efficiency of Membrane Technology Activated Charcoal and a Clay Micelle Complex forthe Removal of Ibuprofen and Mefenamic Acid

Kinetic studies on the stability of two non-steroids anti-inflammatory drugs (NSAIDs), ibuprofen and mefenamic acid, in pure water and activated sludge indicated that both pharmaceuticals were resistant to degradation for one month. The efficiency of sequential advanced membrane technology wastewater treatment plant towards removal of both drugs from wastewater was investigated. The sequential system included activated sludge, ultrafiltration (hollow fiber membranes with 100 kDa cutoff, and spiral wound membranes with 20 kDa cutoff), activated carbon column and reverse osmosis (RO). The overall performance of the integrated plant demonstrated complete removal of ibuprofen and mefenamic acid from spiked wastewater samples. Activated carbon column was the most effective component in removing these NSAIDs with a removal efficiency of 98.8% for both ibuprofen and mefenamic acid. Batch adsorption of both NSAIDs by activated charcoal and a composite micelle (octadecyltrimethylammonium (ODTMA)–clay (montmorillonite) was determined at 25 ˚C. The results revealed that both adsorptions fit Langmuir isotherm with Qmax of 66.7 mg/g and 62.5 mg/g for ibuprofen using activated carbon and clay-micelle complex, respectively, and with Qmax of 90.9 mg/g and 100.0 mg/g for mefenamic acid using activated charcoal and claymicelle complex, respectively. These results suggest that an integration of ODTMA-clay-micelle complex column in wastewater treatment plant is highly promising and can lead to an improvement of the removal efficiency of these drugs from wastewater

Development and Validation of a Stability-Indicating HPLC Method for the Simultaneous Determination of Florfenicol and Flunixin Meglumine Combination in an Injectable Solution

Thecombination of the powerful antimicrobial agent florfenicol and the nonsteroidal anti-inflammatory flunixin meglumine is used for the treatment of bovine respiratory disease (BRD) and control of BRD-associated pyrexia, in beef and nonlactating dairy cattle. This study describes the development and validation of an HPLC-UVmethod for the simultaneous determination of florfenicol and flunixin, in an injectable preparation with a mixture of excipients.The proposed RP-HPLC method was developed by a reversed phase- (RP-) C18e (250mm× 4.6 mm, 5 m) column at roomtemperature, with an isocraticmobile phase of acetonitrile and water mixture, and pH was adjusted to 2.8 using diluted phosphoric acid, a flow rate of 1.0 mL/min, and ultraviolet detection at 268 nm. The stability-indicating method was developed by exposing the drugs to stress conditions of acid and base hydrolysis, oxidation, photodegradation, and thermal degradation; the obtained degraded products were successfully separated from the APIs. This method was validated in accordance with FDA and ICH guidelines and showed excellent linearity, accuracy, precision, specificity, robustness, LOD, LOQ, and system suitability results within the acceptance criteria.This research was supported by the Advanced Veterinary Manufacturing Company (Palestine)

Analysis of Different Rare Metals, Rare Earth Elements, and other Common Metals in Groundwater of South West Bank/Palestine by ICP/MS-Data and Health Aspects

Ground water samples are collected from south West Bank/Palestine and analyzed for different rare elements (Rb, Zr, U, P, Ti, V), rare earth elements (La, Ce, and Nd), and other common trace metals (Li, Na, Mg, Ca, Sr, Ba, K, Bi) that most of them usually have no maximum acceptable limits as either they are considered not to be toxic to human health or there is no sufficient data about their toxicity to human health. This study was conducted to determine the water quality of ground water which is used for drinking in the study area. Water samples from ten groundwater wells were obtained in three different dates of the year (November 2012, March 2013, and April 2013). Three water samples were obtained from each well for each sampling date; so a total of 90 water samples were collected from the ten wells. The results obtained from this study suggest a possible risk to the population of the study area given the high concentration of some metals that have no maximum allowed concentration, and the fact that for many people in the study area, ground water is a main source of their water supply.The authors are grateful for the German research funding organisation (Deutsche Forschungsgemeinschaft), DFG for their financial support through TRION project

Method development and validation of simultaneous determination of seventeenmetals in water by ICP/MS

A simple, precise, accurate, and sensitive method is developed and validated for simultaneous determination of seventeen metals (Li, Sr, Ba, Tl, Pb, Bi, Al, K, Cr, Mn, Co, Ni, Cu, Zn, Mo, Ag, and Cd) in water by ICP-MS. The optimum conditions of the ICP-MS are as follows: nebulizer gas (argon) flow rate: 0.9 L/min, auxiliary gas (argon) flow 0.3 L/min, plasma (argon) gas flow: 15 L/min, reaction gas flow (helium) 4mL/min. This method is validated according to the requirements for new methods, which include linearity and range, accuracy, precision, selectivity, limit of detection (LOD), and limit of quntitation (LOQ). The current method demonstrates good linearity over the range of 1-1000 ppb with r2 greater than 0.999 for the seventeen metals. The recovery of the metals from water samples ranges from 97.5 to 101.7%. The method is selective where minimal interferences between the metals is observed (CeO/Ce = 1%, and Ce+2/Ce+1 = 1%), and with good resolution (0.8 amu at 10% height). The method is also precise where the RSD of the responses (cps) of replicates of the metals at three concentration levels is less than 1%. Low LOD and LOQ of metals using this method enable the detection and quantitation of these metals at low concentrations. Real water samples from West Bank in Palestine (groundwater) were analyzed for their trace metals content using this method

Development and Validation of a Reversed-Phase HPLC Method for Determination of Elaidic Acid in Oils and Fats

A simple, precise, accurate, and selective method with low limit of quantitation (LOQ) was developed and validated for analysis of elaidic acid which is the predominant trans fatty acids in partially hydrogenated vegetable oils. Separation was achieved on a reversed-phase C18 column, using mobile phase consisting of acetonitrile/water (80:20, v/v) containing 0.1% acetic acid, and using UV detection at 205 nm. This method was validated according to the requirements for new methods, which include accuracy, precision, selectivity, robustness, limit of detection (LOD), LOQ, linearity and range. The current method demonstrates good linearity over the range of 3-1000 mg L-1 of elaidic acid with r2 greater than 0.999. The recovery of elaidic acid in oils and fats ranges from 94.5 to 98.7%. The method is selective where elaidic acid is good separated from oleic acid and other components of fats and oils with good resolution. The method is also precise where the RSD of the peak areas of replicate injections of elaidic acid solution is less than 1%. The degree of reproducibility of the results obtained as a result of small deliberate variations in the method parameters and by changing analytical operators has proven that the method is robust and rugged

Development and Validation of a Reversed-Phase HPLC Method for Determination of Elaidic Acid in Oils and Fats

A simple, precise, accurate, and selective method with low limit of quantitation (LOQ) was developed and validated for analysis of elaidic acid which is the predominant trans fatty acids in partially hydrogenated vegetable oils. Separation was achieved on a reversed-phase C18 column, using mobile phase consisting of acetonitrile/water (80:20, v/v) containing 0.1% acetic acid, and using UV detection at 205 nm. This method was validated according to the requirements for new methods, which include accuracy, precision, selectivity, robustness, limit of detection (LOD), LOQ, linearity and range. The current method demonstrates good linearity over the range of 3-1000 mg L-1 of elaidic acid with r2 greater than 0.999. The recovery of elaidic acid in oils and fats ranges from 94.5 to 98.7%. The method is selective where elaidic acid is good separated from oleic acid and other components of fats and oils with good resolution. The method is also precise where the RSD of the peak areas of replicate injections of elaidic acid solution is less than 1%. The degree of reproducibility of the results obtained as a result of small deliberate variations in the method parameters and by changing analytical operators has proven that the method is robust and rugged