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  • A new approach for automated liquid-liquid extraction in a sequential injection manifold.

A new approach for automated liquid-liquid extraction in a sequential injection manifold.

Analytical and bioanalytical chemistry (2014-11-06)
Irene Delgado-Blanca, Eulogio J Llorent-Martínez, Antonio Ruiz-Medina, Pilar Ortega-Barrales
ABSTRACT

A new approach for the implementation of liquid-liquid extraction in a sequential injection manifold is presented. The manifold consists of two syringe pumps and one multi-position valve. The use of a 30 % MeOH/H2O (v/v) solution as the carrier, with isobutanol as the extractant, made it possible to avoid the problems associated with the different affinities of the organic and aqueous phases for Teflon tubing, and the formation of bubbles. The suitability of the proposed method was demonstrated by the determination of thiamine in pharmaceutical preparations and dietary supplements. Detection and quantification limits were estimated as 9 and 30 μg L(-1), respectively. The repeatability was lower than 3 % and the intermediate precision (3 d) was lower than 7 %. The sample throughput was 14 samples per h. The results were in agreement with a high-performance liquid chromatography-electrospray/mass spectrometry reference method.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Chloroform, anhydrous, contains amylenes as stabilizer, ≥99%
Supelco
Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
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Thiamine hydrochloride, ≥98%, FCC, FG
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Chloroform, anhydrous, ≥99%, contains 0.5-1.0% ethanol as stabilizer
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Thiamine hydrochloride, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture
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Supelco
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2-Methyl-1-propanol, BioUltra, Molecular Biology, ≥99.5% (GC)
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Methanol, analytical standard
Supelco
2-Methyl-1-propanol, analytical standard
Sigma-Aldrich
Thiamine hydrochloride, tested according to Ph. Eur.
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
2-Methyl-1-propanol, anhydrous, 99.5%
Sigma-Aldrich
Methanol, purification grade, 99.8%
USP
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2-Methyl-1-propanol, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99% (GC)
Sigma-Aldrich
Thiamine hydrochloride, reagent grade, ≥99% (HPLC)
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Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Chloroform, contains 100-200 ppm amylenes as stabilizer, ≥99.5%
Sigma-Aldrich
2-Methyl-1-propanol, ACS reagent, ≥99.0%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Chloroform, ACS spectrophotometric grade, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Chloroform, contains amylenes as stabilizer, ACS reagent, ≥99.8%