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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

Supelco
Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Chloroform, SAJ super special grade, ≥99.0%
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Chloroform, JIS 300, ≥99.0%, for residue analysis
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Chloroform, suitable for HPLC
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Thiamine hydrochloride, ≥98%, FCC, FG
Supelco
Thiamine Hydrochloride (B1), analytical standard
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Chloroform, analytical standard
Supelco
2-Methyl-1-propanol, analytical standard
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Thiamine hydrochloride, tested according to Ph. Eur.
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Chloroform, anhydrous, contains amylenes as stabilizer, ≥99%
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Chloroform, anhydrous, ≥99%, contains 0.5-1.0% ethanol as stabilizer
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2-Methyl-1-propanol, anhydrous, 99.5%
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Thiamine hydrochloride, reagent grade, ≥99% (HPLC)
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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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Thiamine hydrochloride, meets USP testing specifications
Supelco
Heptafluorobutyric acid solution, 0.5 M in H2O, LiChropur, suitable for ion pair chromatography
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2-Methyl-1-propanol, suitable for HPLC, 99.5%
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Methanol, ACS reagent, ≥99.8%
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Methanol, suitable for HPLC, gradient grade, ≥99.9%
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Chloroform, puriss. p.a., reag. ISO, reag. Ph. Eur., 99.0-99.4% (GC)
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Chloroform, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains amylenes as stabilizer
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Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
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2-Methyl-1-propanol, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99% (GC)
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Methanol, suitable for HPLC, ≥99.9%
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Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
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Chloroform, contains ethanol as stabilizer, ACS reagent, ≥99.8%
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Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Methanol, HPLC Plus, ≥99.9%
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