Skip to Content
Merck
  • 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
Methanol, NMR reference standard
Supelco
Heptafluorobutyric acid solution, 0.5 M in H2O, LiChropur, suitable for ion pair chromatography
Supelco
Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
2-Methyl-1-propanol, analytical standard
USP
Thiamine hydrochloride, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
2-Methyl-1-propanol, BioUltra, for molecular biology, ≥99.5% (GC)
Supelco
Methanol, analytical standard
Supelco
Thiamine Hydrochloride (B1), analytical standard
Sigma-Aldrich
2-Methyl-1-propanol, anhydrous, 99.5%
Sigma-Aldrich
Thiamine hydrochloride, ≥98%, FCC, FG
Sigma-Aldrich
Thiamine hydrochloride, tested according to Ph. Eur.
Sigma-Aldrich
Thiamine hydrochloride, reagent grade, ≥99% (HPLC)
Sigma-Aldrich
Thiamine hydrochloride, meets USP testing specifications
Sigma-Aldrich
Thiamine hydrochloride, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture
Sigma-Aldrich
Chloroform, ≥99%, PCR Reagent, contains amylenes as stabilizer
Supelco
Chloroform, analytical standard
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Chloroform, biotech. grade, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Chloroform, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Chloroform, suitable for HPLC, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Chloroform, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains amylenes as stabilizer
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Mesalazine for system suitability, European Pharmacopoeia (EP) Reference Standard
Supelco
Chloroform, Pharmaceutical Secondary Standard; Certified Reference Material
Thiamine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Chloroform, contains ethanol as stabilizer, ACS reagent, ≥99.8%