Determination of Tin in Canned Fruits and Vegetables by Atomic Absorption Spectrometry and Liquid–Liquid Extraction

1994 ◽  
Vol 77 (6) ◽  
pp. 1627-1630 ◽  
Author(s):  
Ana M Martín ◽  
Mercedes Sánchez ◽  
Pedro Espinosa ◽  
Gracia Bagur

Abstract A method was developed for the determination of tin based on the extraction of its 5,5-methylenedisalicylohydroxamic acid complex with 1.09M isobutyl methyl ketone in tributyl phosphate. After the samples were treated with nitric and hydrochloric acid, the aqueous phase was made to 0.05M in perchloric acid. When the ratio of aqueous phase to organic phase was 4:1 (v/v), the detection limit and the relative standard deviation (n = 7,50 μg tin) were 0.20 μg/mL and 0.9%, respectively. The proposed method was applied to the analysis of tin in canned fruits and vegetables. The results were in good agreement with those obtained by the phenylfluorone method.

2011 ◽  
Vol 47 (2) ◽  
pp. 363-371 ◽  
Author(s):  
Ananda Lima Sanson ◽  
Suéllen Cristina Rennó Silva ◽  
Matheus Coutinho Gonçalves Martins ◽  
Alexandre Giusti-Paiva ◽  
Patrícia Penido Maia ◽  
...  

A liquid-liquid extraction (LLE) combined with high-performance liquid chromatography-diode array detection method for simultaneous analysis of four chemically and structurally different antineoplastic drugs (cyclophosphamide, doxorubicin, 5-fluorouracil and ifosfamide) was developed. The assay was performed by isocratic elution, with a C18 column (5 µm, 250 x 4.6 mm) and mobile phase constituted by water pH 4.0- acetonitrile-methanol (68:19:13, v/v/v), which allowed satisfactory separation of the compounds of interest. LLE, with ethyl acetate, was used for sample clean-up with recoveries ranging from 60 to 98%. The linear ranges were from 0.5 to 100 µg mL-1, for doxorubicin and 1 to 100 µg mL-1, for the other compounds. The relative standard deviations ranged from 5.5 to 17.7%. This method is a fast and simple alternative that can be used, simultaneously, for the determination of the four drugs in plasma, with a range enabling quantification of the drugs in pharmacokinetics, bioequivalence and therapeutic drug-monitoring studies.


1983 ◽  
Vol 66 (4) ◽  
pp. 850-852
Author(s):  
Earle E Cary ◽  
Michael Rutzke

Abstract This method involves sample digestion in nitric, perchloric, and sulfuric acids. Chromium is concentrated by coprecipitation with ferric hydroxide. Redissolved iron is removed by liquid-liquid extraction, remaining silica is dissolved with hydrofluoric acid, and chromium is determined by electrothermal atomic absorption spectrometry. The sensitivity and detection limits for chromium approach those given by the manufacturers of the various instruments. Recovery studies and analysis of standard materials show that this method is reliable.


1999 ◽  
Vol 82 (6) ◽  
pp. 1436-1442 ◽  
Author(s):  
Oroncio Jiménez de Blas ◽  
Josë Luis Pereda de Paz

Abstract We developed a new procedure for the indirect determination of the organophosphorus pesticide dimethoxydithiophosphate (DDTP) by coupling, in continuous mode, flow injection analysis (FIA) with liquid-liquid extraction and atomic absorption spectrometry with hydride generation in the organic phase. Both continuous-mode extraction of the species Bi(DDTP)3 in isobutylmethylketone (IBMK) organic medium and the process of hydride(BiH3) generation in the same organic medium were optimized. The most suitable solvent of the reducing agent, NaBH4, was a 1 % solution of N,N-dimethylformamide in glacial acetic acid medium. Phase separation was accomplished with an original design that has been patented for use (Spain patent 10,118,929 Y). The hydride generated is transported by the FIA setup in continuous mode to the quartz cell where the analytical signal was measured. The procedure developed was rapid, continuous, and involved little manipulation, thus avoiding possible errors and contamination. Moreover, only small amounts (250 μL) of sample were required in the injection of the aqueous sample, and a volume of 30 μL was used in the injection of the organic phase extracted. The values obtained for the detection limit (5 ppb DDTP in the aqueous phase injected) and for precision (3.0%, expressed as coefficient of variation) are very acceptable in comparison with other procedures described in the literature. The accuracy obtained was in agreement with the imprecision of the method when it was applied to the aqueous samples. The procedure can be used for the analysis of surface waters subject to different types of treatment prior to their use for human consumption. For this type of water, European legislation permits pesticide concentrations up to 5 ppb, which is the value of the detection limit obtained in the proposed procedure.


2014 ◽  
Vol 68 (3) ◽  
Author(s):  
Samat Kinaree ◽  
Saksit Chanthai

AbstractThe determination of Pb(II) and Cd(II) in different sample matrices, including drinking water, distilled spirits and fruit wine, was carried out by flame atomic absorption spectrometry (FAAS) after pre-concentration using homogeneous liquid-liquid extraction (HLLE). First, the HLLE method was optimised with lead diethyldithiocarbamate (Pb-DDTC) complex which was extracted with a perfluorooctanoate anion (PFOA−) dissolved in lithium hydroxide under acidic conditions. The optimum extraction conditions, using 0.01 M DDTC, 0.05 M PFOA−, 3 M HCl and 1 mL of 30 vol. % acetone, were obtained. The Pb-DDTC complex in the nitric acid digest of the samples (50–150 mL) was extracted quantitatively into a drop of 100 μL of sediment phase. The sediment phase dissolved in 1 vol. % HNO3 with at least 3–5 mL of the final volume was then determined by FAAS, affording a pre-concentration factor of 10–50. Hence, the HLLE method afforded an increase in both sensitivity and selectivity for the metal determination by conventional FAAS, resulting in ultra-trace level detection of Pb(II) in all samples analysed (drinking water, 9.2–23 ng mL−1; distilled spirits, 23–50 ng mL−1; fruit wine, 24–53 ng mL−1). In addition, the proposed method could successfully be applied to Cd(II) determination in these samples.


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