Fast gas chromatography with solid phase extraction clean-up for ultratrace analysis of pesticide residues in baby food.

A sample preparation method based on single solvent phase extraction and solid-phase extraction (SPE-NH2) clean-up is studied in combination with fast capillary gas chromatography (GC) to determine 18 selected pesticides belonging to various chemical classes in apples, the common raw material for baby food production and baby food, at the concentration level < or = 10 microg/kg maximum residual limit (MRL). Possibilities of mass spectrometry (MS) detector and electron capture detector (ECD) in fast gas chromatography (GC) of samples with complex matrice at ultra trace levels of pesticide residues were studied and compared. MS detection in single ion monitoring (SIM) mode provided higher selectivity compared to ECD. Optimisation of extraction as well as the simplifying of the whole process of sample preparation was carried out. Recoveries obtained at concentration level of 5 microg/kg (the required value for limit of quantification (LOQ) in baby food) were >90%, except of dimethoate (77.7%) and captan (46.4%) with MS detection. The obtained LOQs were at least 1 order lower than 5 microg/kg for the majority of compounds. The repeatability of gas chromatography-mass spectrometry (GC-MS) measurements of the matrix matched standards expressed as relative standard deviation was <11% except of captan and cypermethrin.

Isotachophoretic determination of naproxen in the presence of its metabolite in human serum.

An isotachophoretic method with conductivity detection was developed to determine naproxen in the presence of its metabolite 6-O-desmethylnaproxen in human serum. The leading electrolyte contained 10 mM hydrochloric acid, beta-alanine, pH 4.0 and 0.1% methylhydroxypropylcellulose. The terminating electrolyte was 10 mM 2-(N-morpholino)ethanesulfonic acid-tris(hydroxymethyl)aminomethane, pH 6.9, containing 20% (v/v) of ethanol. Naproxen was determined in serum supernatant after simple deproteination of the sample with ethanol. The isotachophoretic results were compared with those obtained by synchronous fluorescence spectrometry.

Determination of ibuprofen and naproxen in tablets.

Ibuprofen and naproxen have been quantified in tablets by capillary isotachophoresis. Hydrochloric acid (10 mmol/l) adjusted with creatinine to pH 5.0 plus 0.1% polyvinylpyrrolidone was used as the leading electrolyte and 10 mmol/l 4-morpholineethanesulfonic acid as the terminating electrolyte. Linearity was observed from 40.0 to 200.0 mg/l of ibuprofen (naproxen), with a coefficient of determination (r2) of 0.999. Good quantitation was obtained in short analysis time. The isotachophoretic results were compared with those obtained by the fluorescence spectrometry. Experimental parameters for ibuprofen were: lambdaEX=224 nm and lambdaEM=290 nm. Experimental parameters for naproxen were: lambdaEX=230 nm and lambdaEM=355 nm. The calibration plot was found to be linear in the range 0.4-2.4 mg/l for ibuprofen and 5.0-20.0 microg/l for naproxen. The minimal sample pretreatment and relatively low running cost make isotachophoresis a good alternative to existing methods.

Determination of some antirheumatics by capillary isotachophoresis.

Isotachophoresis (ITP) was applied for the determination of some antirheumatic drugs (fenoprofen, naproxen, ibuprofen, and ketoprofen) in human serum. The leading electrolyte contained hydrochloric acid (10 mmol x L(-1)), creatinine (pH 4.5) and methylhydroxyethyl cellulose (0.1%). The terminating electrolyte was 2-(N-morpholino)ethanesulfonic acid (10 mmol x L(-1)) adjusted with tris(hydroxymethyl)aminomethane to pH 6.9. The ITP separations were carried out in column-coupling configuration of the separation unit provided with a preseparation column of 160 x 0.8 mm inner diameter (ID) and analytical column of 160 x 0.3 mm ID. The limit of detection for ibuprofen, fenoprofen, and naproxen in serum by direct sampling was 0.008, 0.005 and 0.004 mmol x L(-1). The limit of detection for ketoprofen in serum after ethanol precipitation was 0.001 mmol x L(-1).

Determination of non-steroidal anti-inflammatory drugs in biological fluids.

The present paper summarizes the methods of determination of non-steroidal anti-inflammatory drugs in biological fluids. CZE, HPLC, HPTLC, GC-MS are analytical techniques, which are capable of a separation of arylpropionic acids.

Determination of fenoprofen in serum by capillary isotachophoresis.

A isotachophoretic method with conductivity detection was developed and validated to directly determine fenoprofen in human serum. The leading electrolyte contained hydrochloric acid (10 mmol/l), 6-aminocaproic acid (pH 4.8) and polyvinylpyrrolidone (0.1%). The terminating electrolyte was 4-morpholineethanesulfonic acid (5 mmol/l). The calibration curve was linear over the concentration range 0.02-0.40 mmol/l. Within-day standard deviation ranged from 0.001 to 0.004 and between-day standard deviation ranged from 0.001 to 0.004. The limit of determination was 0.02 mmol/l. The assay was employed to determine serum concentration of fenoprofen in patients.

Isotachophoretic determination of bisoprolol, clonidine, disopyramide and tolazoline in human fluids.

Separation and determination of bisoprolol, clonidine, disopyramide and tolazoline in control serum and in human urine was investigated by capillary isotachophoresis. The drugs were separated by using the cationic electrolyte system. viz., sodium acetate buffer (pH 4.64) (c1 = 10 mM)-beta-alanine. The compounds were almost totally isolated from serum by solid-phase extraction using a Sep-Pak C18 cartridge. The recovery of compounds varied from 87 to 99%. The linear calibration range was studied to apply the method to real human fluids. The limit of determination of the drugs was 40.0 micrograms/ml serum. The limit of determination by direct sampling for bisoprolol is 3 micrograms/ml urine.