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EN
A convenient method was developed for simultaneous determination of 11 preservatives in cosmetics and pharmaceuticals. Matrix solid-phase dispersion had been optimized as the sample pretreatment technology, using Florisil as a dispersant, anhydrous sodium sulfate as a dehydrant, formic acid as an additive, and n-hexane and ethyl acetate as eluents successively, and followed by gas chromatography–flame ionization detection on a TR-5 capillary column. Experimental results showed that 11 preservatives were baseline separated within 22 min. Good linearities were observed in the concentration range of 0.53–250 μg/mL for all analytes, and there were also minor differences. All correlation coefficients (r) were more than 0.995. The average recoveries at 3 levels of spiked samples ranged from 80% to 124% with 0.9–12% intra-day RSD and 1.8–12% inter-day RSD. The limits of detection were less than 0.18 μg/mL for all analytes. Besides, there was no obvious matrix effect on the analytes. The conclusion was that the developed method was simple, cheap, accurate, precise, and environment-friendly, in addition to existing little matrix effects. It could be recommended to determine 11 preservatives individually or in any their combinations to not only in liquid and gel cosmetics but also in liquid medicine and ointment.
EN
A rapid and simple analytical method based on matrix solid-phase dispersion combined with liquid chromatography coupled with tandem mass spectrometry has been developed by using bamboo charcoal as a dispersive adsorbent to simultaneously determine tetrabromobisphenol A (TBBPA) and hexabromocyclododecane diastereoisomers (HBCDs) in soil. The factors influencing the performance of the proposed method were investigated and optimized in detail, and the matrix effects were evaluated. Under optimum conditions, the proposed method showed good linearity within the range of 0.8–80 ng g−1 and limits of detection of 4–75 pg g−1 (S/N = 3). The satisfactory recoveries of TBBPA ranging from 72.8% to 92.5% and HBCDs ranging from 76.8% to 102.2% were obtained with relatively standard deviation (RSD) ranging from 3.4% to 9.8%. The proposed method has been successfully applied to analyze TBBPA and HBCDs in actual soil samples from the Yellow River Delta in China.
EN
The use of matrix solid-phase dispersion (MSPD) was tested to extract some coumarins (umbelliferone, xanthotoxin, isopimpinellin, bergapten, and pimpinellin) from Pimpinella roots. The method was compared with liquid—solid extraction methods (LSE) such as accelerated solvent extraction (ASE), ultrasound-assisted extraction (USAE) and Soxhlet extraction followed by solid-phase extraction (SPE). Several methanol concentrations and temperature conditions were examined during the liquid—solid extraction techniques. The analysis was performed by high-performance liquid chromatography with diode array detector (HPLC—DAD). MSPD extracted furanocoumarins with satisfactory recoveries ranging from 91.65% to 97.55% and relative standard deviations lower than 5,0415%. The results presented in the paper reveal that MSPD is an efficient, fast, simple and easy-to-perform method suitable for the isolation of furanocoumarins from herbs.
EN
The matrix solid-phase dispersion (MSPD) method with GC detection for the determination of of residues of fourteen fungicides (azoxystrobin, bitertanol, bupirimate, captan, chlorothalonil, dichlofluanid, fenarimol, flusilazole, iprodione, metalaxyl, procymidone, pyrimethanil, tetraconazole, vinchlozolin) that are currently applied lo agricultural crops is described. The method uses Florisil and silica as MSPD sorbents. Different parameters, such as type of solid phase, eluting solvent and matrix, were investigated. Recovery checks have been carried out on different commodities (tomatoes, cucumbers, strawberries, apples, raspberries, and melons). The limits of detection were in the 0.003-0.01 mg kg(1) range and were about 10 times lower than the maximum residue limits allowed. Compared with classical methods, the procedure described is simple, rapid and economical, and may be useful for the determination of fungicides of different chemical structures. These pesticides have been detected in samples taken from the fields at levels of 0.006-4.295 mg kg(-1).
PL
Opisano metodę rozproszenia matrycy w fazie stałej (MSPD) z detekcją GC w zastosowaniu do oznaczania pozostałości czternastu fungicydów (azoksystrobiny, hitertanolu, bupirymatu, chlorotalonilu, dichlofluanidu, fenaritnolu, flusilazolu, iprodionu. kaptanu, metalaksylu, pirymetanilu, procymidonu, tetrakonazolu, winchlozoliny), które są obecnie stosowane w rolnictwie do ochrony owoców i warzyw przed chorobami grzybowymi. W metodzie użyto Florisilu i żelu krzemionkowego jako adsorbentów. Badano parametry, takiejak typ fazy stałej, eluent i rodzaj matrycy. Odzysk metody sprawdzano na próbkach różnych owoców i warzyw (pomidory, truskawki, jabłka, maliny i melony). Wykrywalność oznaczanych związków mieściła się w zakresie 0.003-0.01 mg kg(1) i była około 10 razy niższa niż ich najwyższy dopuszczalny poziom. W porównaniu z metodami klasycznymi, opisana procedura jest prosta, szybka, ekonomiczna i może być używana do oznaczania tungicydów o różnych strukturach chemicznych. Pestycydy w próbkach pobranych z pól wykrywano w zakresie 0.006-4.295 mg kg(-1).
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