Sensitive determination of atorvastatin in human plasma by dispersive liquid-liquid microextraction and solidification of floating organic drop followed by high-performance liquid chromatography.

A novel and sensitive dispersive liquid-liquid microextraction method based on the solidification of the floating organic drop combined with high-performance liquid chromatography and ultraviolet detection was used for the determination of atorvastatine in blood serum samples. The chromatographic separation of atorvastatin was carried out using methanol as the mobile phase organic modifier. Various parameters affecting the extraction efficiency were optimized, such as the kind and volume of extraction solvent (1-undecanol) and disperser solvent (acetonitrile), pH, and the extraction time. The calibration curve was linear in the range of 0.2-6000 μg/L of atorvastatin (r(2) = 0.995) with a limit of detection of 0.07 μg/L. The relative standard deviation for 100 μg/L of atorvastatin in human plasma was 8.4% (n = 4). The recoveries of plasma samples spiked with atorvastatin were in the range of 98.8-113.8%. The obtained results showed that the proposed method is fast, simple, and reliable for the determination of very low concentrations of atorvastatin in human plasma samples.

Taheri S ，Jalali F ，Fattahi N ，Bahrami G ... -  《-》

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection to determination of opium alkaloids in human plasma.

A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma.

Ahmadi-Jouibari T ，Fattahi N ，Shamsipur M ，Pirsaheb M ... -  《-》

Rapid extraction and determination of amphetamines in human urine samples using dispersive liquid-liquid microextraction and solidification of floating organic drop followed by high performance liquid chromatography.

A novel, rapid, simple and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine amphetamine and methamphetamine in urine samples. The factors affecting the extraction efficiency of DLLME-SFO such as the kind and volume of the extraction and the disperser solvents, effect of concentration of K2CO3 and extraction time were investigated and the optimal extraction conditions were established. Under the optimum conditions (extraction solvent: 30.0μl 1-undecanol; disperser solvent: 300μl acetonitrile; buffer concentration: 2% (w/v) K2CO3 and extraction time: 1min), calibration curves are linear in the range of 10-3000μgl(-1) and limit of detections (LODs) are in the range of 2-8μgl(-1). The relative standard deviations (RSDs) for 100μgl(-1) of amphetamine and methamphetamine in diluted urine are in the range of 6.2-7.8% (n=7). The method was successfully applied for the determination of amphetamine and methamphetamine in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 87.8-113.2%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of amphetamine and methamphetamine in urine.

Ahmadi-Jouibari T ，Fattahi N ，Shamsipur M 《-》

Low-density solvent-based dispersive liquid-liquid microextraction combined with single-drop microextraction for the fast determination of chlorophenols in environmental water samples by high performance liquid chromatography-ultraviolet detection.

A new format of fast three-phase microextraction by combining low-density solvent-based dispersive liquid-liquid microextraction (DLLME) and single-drop microextraction (SDME) was for the first time developed for the determination of chlorophenols in environmental water samples. The extraction procedure includes a 2 min DLLME pre-extraction and a 10 min SDME back-extraction. A portion of low-density solvent (toluene) was used as organic phase and injected into the aqueous sample (donor phase) with methanol as disperser. The analytes were pre-extracted into the organic phase within 2 min. A thin layer of the organic phase formed on the top of the aqueous phase by a 2 min centrifugation. Then a drop of acceptor solution was introduced into the upper layer and SDME was carried out for the back-extraction. The stirring step typically involved in SDME and LLLME is avoided with the benefit of the high speed and efficiency of DLLME pre-extraction. After extraction, the acceptor drop was withdrawn and directly injected into a high performance liquid chromatography instrument with ultraviolet detection for analysis. Five chlorophenols, 4-chlorophenol, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, and pentachlorophenol, were selected as model compounds for developing and evaluating the method. Factors affecting extraction efficiency were studied, including the organic solvent, the disperser solvent, the composition of donor phase and acceptor phase, the volume of acceptor microdrop, and the extraction time. At optimal conditions, the method showed low detection limit (0.016-0.084 μg/L) for the five chlorophenols, good linearity (from 0.2-250 to 1.0-250 μg/L, depending on the analytes) and repeatability (RSD below 8.2, n=5). The simple, fast, and efficient feature of the proposed method was demonstrated by the analysis of chlorophenols in environmental water samples.

Li X ，Xue A ，Chen H ，Li S ... -  《-》

Dispersive liquid-liquid microextraction based on solidification of floating organic drop and high-performance liquid chromatography to the analysis of cocaine's major adulterants in human urine.

A simple method has been proposed for the determination of cocaine's major adulterants (caffeine, levamisole, lidocaine, phenacetin, diltiazem, and hydroxyzine) in human urine by dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) in combination with high-performance liquid chromatography - photodiode array detector (HPLC-PDA). The reversed-phase chromatographic separation was obtained with a column C18 extended (250×4.6mm; 5μm; 80Å) in gradient elution mode using acetonitrile-trifluoroacetic acid 0.026% (v,v) (pH=2.5) at 1mLmin-1 as mobile phase, at 25°C, and detection at 235nm. The analysis time was 25min. This condition had the best resolution factors (>1.15), retention factors (>0.68), number of plates (>2094.9), and separation factors (>1.05) for all targets, indicating a good separation. The kind of extraction and dispersive solvent were investigated for unifactorial design. The buffer pH, the volume of extraction and disperser solvent, and the amount of salt were optimized for full factorial design. Under optimum conditions, human urine samples were alkalized with 0.5M sodium phosphate buffer (pH 10) and added to sodium chloride (20%m/v). Acetonitrile (150μL) and 1-dodecanol (30μL) were used as dispersive and extraction solvent, respectively. The method presented linear range of 312.5-3125ngmL-1 to caffeine and levamisole and 187.5-1875ngmL-1 to lidocaine, phenacetin, diltiazem, and hydroxyzine. The limit of quantification was 187.5ngmL-1 to lidocaine, phenacetin, diltiazem, and hydroxyzine and 312.5ngmL-1 for caffeine and levamisole. The recovery mean values were between 6.0 and 42.6%. The method showed good precision and accuracy, with within- and between-run relative standard deviation and relative error less than 15%. The samples were stable after freeze-thaw cycle and short-term room temperature stability tests. Besides, this method was satisfactorily applied in urine of cocaine users. It is expected that this method, which was the first to combine the use of DLLME-SFO and HPLC-PDA for the determination of cocaine's major adulterants in human urine, will contribute to the accuracy in the diagnosis of acute intoxication, the proper planning of therapeutic measures, as well as to the favorable prognostic of cocaine intoxicated patients.

Sena LC ，Matos HR ，Dórea HS ，Pimentel MF ，de Santana DC ，de Santana FJ ... -  《-》