Microextraction Techniques for Sample Preparation of Amphetamines in Urine: A Comprehensive Review.

Psychological disorders and dramatic social problems are serious concerns regarding the abuse of amphetamine and its stimulant derivatives worldwide. Consumers of such drugs experience great euphoria along with serious health problems. Determination and quantification of amphetamine-type stimulants are indispensable skills for clinical and forensic laboratories. Analysis of low drug doses in bio-matrices necessitates applications of simple and also effective preparation steps. The preparation procedures not only eliminate adverse matrix effects, but also provide reasonable clean-up and pre-concentration benefits. The current review presents different methods used for sample preparation of amphetamines from urine as the most frequently used biological matrix. The advantages and limitations of various sample preparation methods were discussed focusing on the miniaturized methods.

Determination of Organothiophosphate Insecticides in Environmental Water Samples by a Very Simple and Sensitive Spectrofluorimetric Method.

A simple, rapid and sensitive spectrofluorimetric method was developed for the determination of di-syston, ethion and phorate in environmental water samples. The procedure is based on the oxidation of these pesticides with cerium (IV) to produce cerium (III), and its fluorescence was monitored at 368 ± 3 nm after excitation at 257 ± 3 nm. The variables effecting oxidation of each pesticide were studied and optimized. Under the experimental conditions used, the calibration graphs were linear over the range 0.2-15, 0.1-13, 0.1-13 ng mL(-1) for di-syston, ethion and phorate, respectively. The limit of detection and quantification were in the range 0.034-0.096 and 0.112-0.316 ng mL(-1), respectively. Intra- and inter-day assay precisions, expressed as the relative standard deviation (RSD), were lower than 5.2 % and 6.7 %, respectively. Good recoveries in the range 86 %-108 % were obtained for spiked water samples. The proposed method was applied to the determination of studied pesticides in environmental water samples.

Analysis of piroxicam in pharmaceutical formulation and human urine by dispersive liquid-liquid microextraction combined with spectrophotometry.

PURPOSE: Piroxicam, is non-steroidal anti-inflammatory and analgesic agent, which is widely used in the treatment of patients with rheumatologic disorders. A new analytical approach based on the dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and determination of PX in pharmaceutical preparation and human urine. METHODS: From the PX standard solution or solutions prepared from real samples, aliquot volumes were pipetted into centrifuge tubes and mixed with acetate buffer at pH 3.0 and NaCl solution. The contents were subjected to the DLLME, so 700 µL of methanol containing 70 µL of chloroform was injected rapidly into a sample solution. A cloudy solution was rapidly produced and the PX extracted into dispersed fine droplets. The mixture was centrifuged, thus these fine droplets of chloroform were settled. The supernatant aqueous phase was readily decanted, then the remained organic phase was diluted with ethanol and the absorbance measured at 355 ± 3 nm against a reagent blank. RESULTS: The main factors affecting the extraction efficiency such as pH, extraction and disperser solvent types and etc. were studied and optimized systematically. Under optimized conditions, the calibration graphs were linear over the range of 0.2 to 4.8 µg/mL. The limit of detection and relative standard deviation were found to be 0.058 µg/mL and 2.83%, respectively. Relative recoveries in the spiked samples ranged from 97 to 110%. CONCLUSION: Using the developed method PX can be analyzed in pharmaceutical formulation and human urine sample in a simpler, cheaper and more rapid manner.

Development of a dispersive liquid-liquid microextraction technique for the extraction and spectrofluorimetric determination of fluoxetine in pharmaceutical formulations and human urine.

PURPOSE: Fluoxetine is the most prescribed antidepressant drug worldwide. In this work, a new dispersive liquid-liquid microextraction (DLLME) method combined with spectrofluorimetry has been developed for the extraction and determination of FLX in pharmaceutical formulations and human urine. METHODS: For FLX determination, the pH of a 10 mL of sample solution containing FLX, was adjusted to 11.0. Then, 800 µL of ethanol containing 100 µL of chloroform was injected rapidly into the sample solution. A cloudy solution was formed and FLX extracted into the fine droplets of chloroform. After centrifugation, the extraction solvent was sedimented and supernatant aqueous phase was readily decanted. The remained organic phase was diluted with ethanol and its fluorescence was measured at 292±3 nm after excitation at 234±3 nm. RESULTS: Some important parameters influencing microextraction efficiency were investigated. Under the optimum extraction conditions, a linear calibration curve in the range of 10 to 800 ng/mL with a correlation coefficient of r(2) = 0.9993 was obtained. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 2.78 and 9.28 ng/mL, respectively. The relative standard deviations (RSDs) were less than 4%. Average recoveries for spiked samples were 93-104%. CONCLUSION: The proposed method gives a very rapid, simple, sensitive, wide dynamic range and low-cost procedure for the determination of FLX.