Parallel artificial liquid membrane extraction of acidic drugs from human plasma.

The new sample preparation concept "Parallel artificial liquid membrane extraction (PALME)" was evaluated for extraction of the acidic drugs ketoprofen, fenoprofen, diclofenac, flurbiprofen, ibuprofen, and gemfibrozil from human plasma samples. Plasma samples (250 µL) were loaded into individual wells in a 96-well donor plate and diluted with HCl to protonate the acidic drugs. The acidic drugs were extracted as protonated species from the individual plasma samples, through corresponding artificial liquid membranes each comprising 2 µL of dihexyl ether, and into corresponding acceptor solutions each comprising 50 µL of 25 mM ammonia solution (pH 10). The liquid membranes and the acceptor solutions were located in a 96-well filter plate, which was sandwiched with the 96-well donor plate during extraction. Parallel extraction of several samples was performed for 15 to 60 min, followed by high-performance liquid chromatography-ultraviolet detection of the individual acceptor solutions. Important PALME parameters including the chemical composition of the liquid membrane, extraction time, and sample pH were optimized, and the extraction performance was evaluated. Except for flurbiprofen, exhaustive extraction was accomplished from plasma. Linearity was obtained for all six drugs in the range 0.025-10 µg/mL, with r (2) values ranging between 0.998 and 1.000. Precision data were in the range 3-22% RSD, and accuracy data were within 72-130% with spiked plasma samples. Based on the current experiences, PALME showed substantial potential for future high-throughput bioanalysis of non-polar acidic drugs.

Stir fabric phase sorptive extraction for the determination of triazine herbicides in environmental waters by liquid chromatography.

Stir fabric phase sorptive extraction (SFPSE), which integrates sol-gel hybrid organic-inorganic coated fabric phase sorptive extraction media with a magnetic stirring mechanism, is presented for the first time. Two flexible fabric substrates, cellulose and polyester were used as the host matrix for three different sorbents e.g., sol-gel poly(tetrahydrofuran), sol-gel poly(ethylene glycol), and sol-gel poly(dimethyldiphenylsiloxane). The new microextraction device has been analytically evaluated using triazine herbicides as model compounds. The factors affecting the extraction efficiency of SFPSE have been investigated and the optimal extraction conditions have been determined. Under these optimum conditions, the limits of quantification (LOQs) for sol-gel poly(ethylene glycol) coated SFPSE device in combination with UPLC-DAD for the analysis of the seven triazine herbicides were in the range of 0. 26-1.50µg/L with precision (relative standard deviation) at 2µg/L concentration ranging from 1.4-4.8% (intra-day, n=5) and 6.8-11.8% (inter-day, n=3). Enrichment factors were found between 444 and 1411 (compared to 2000 theoretical maximum). Absolute extraction recoveries were in the range of 22.2-70.5%. The developed method was applied for the determination of selected triazine herbicides from three river water samples. Relative recoveries of the target analytes, in the range from 75 to 126%, were found to be satisfactory. The combination of SFPSE with LC-MS/MS allows the improvement of the method sensitivity to the range from 0.015µg/L to 0.026µg/L with precision better than 10.8% expressed as relative standard deviation (RSD).

Stir-membrane solid-liquid-liquid microextraction for the determination of parabens in human breast milk samples by ultra high performance liquid chromatography-tandem mass spectrometry.

In this article, stir-membrane solid-liquid-liquid microextraction (SM-SLLME) is tailored for the analysis of solid matrices and it has been evaluated for the determination of parabens in l breast milk samples. A three-phase microextraction mode was used for the extraction of the target compounds taking advantage of their acid-base properties. The unit allows the simultaneous extraction of the target compounds from the solid sample to an organic media and the subsequent transference of the analytes to an aqueous acceptor phase. The method includes the identification and quantification of the analytes by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). All the variables involved in the extraction procedure have been accurately studied and optimized. The analytes were detected and quantified using a triple quadrupole mass spectrometer (QqQ). The selection of two specific fragmentation transitions for each compound allowed simultaneous quantification and identification. The method has been analytically characterized on the basis of its linearity, sensitivity and precision. Limits of detection ranged from 0.1 to 0.2ngmL(-1) with precision better than 8%, (expressed as relative standard deviation). Relative recoveries were in the range from 91 to 106% which demonstrated the applicability of the stir-membrane solid-liquid-liquid microextraction for the proposed analytical problem. Moreover, the method has been satisfactorily applied for the determination of parabens in lyophilized breast milk samples from 10 randomly selected individuals.