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  • A novel miniaturized extraction capillary for determining gaseous formaldehyde by high-performance liquid chromatography.

A novel miniaturized extraction capillary for determining gaseous formaldehyde by high-performance liquid chromatography.

Analytical and bioanalytical chemistry (2014-09-10)
Ikuo Ueta, Suguru Mochizuki, Susumu Kawakubo, Tetsuo Kuwabara, Kiyokatsu Jinno, Yoshihiro Saito
ABSTRACT

A novel miniaturized sample extraction capillary was developed to provide a simple and sensitive method for analyzing gaseous formaldehyde (FA) using conventional high-performance liquid chromatography (HPLC). The extraction capillary was prepared by packing silica gel particles in a stainless steel capillary with a 1.6-mm o.d. Before the gaseous samples were collected, the silica gel particles were impregnated with a derivatizing reagent 2,4-dinitrophenylhydrazine (DNPH) by passing a solution of DNPH through the extraction capillary. FA was derivatized to form the corresponding hydrazone during the active sampling of a gaseous sample, and the derivative was sorbed by the silica gel. The capillary was then directly connected to a six-port valve, and desorption from the capillary and injection into the HPLC were achieved simultaneously by passing a solvent through the capillary. The run-to-run and device-to-device variabilities, as relative standard deviations, were both less than 6.9%. The limit of detection for FA was 2.5 ng/L using a sampling volume of 100 mL, and a sample collection time of 2 min. Acetaldehyde and acetone in a gaseous sample could also be simultaneously extracted and determined using this method. The applicability of the developed method for determining FA in real indoor air samples was confirmed by comparing the results obtained using the proposed method and a conventional sample preparation method. The developed method enables the rapid and simple sample preparation of gaseous FA and gives a good level of sensitivity.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetaldehyde, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
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Hydrogen chloride, ReagentPlus®, ≥99%
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Acetaldehyde, puriss. p.a., anhydrous, ≥99.5% (GC)
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Acetaldehyde, ReagentPlus®, ≥99.0% (GC)
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Formaldehyde-DNPH solution, certified reference material, TraceCERT®, 100 μg/mL in acetonitrile (as aldehyde), ampule of 1 mL
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Formaldehyde-2,4-DNPH, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Acetonitrile, electronic grade, 99.999% trace metals basis
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Ultrapure Acetonitrile
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Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)
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Acetonitrile, for HPLC, for UV, ≥99.9% (GC)
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Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
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Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
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USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
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Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
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Acetonitrile, ReagentPlus®, 99%
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Acetonitrile, for preparative HPLC, ≥99.8% (GC)
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Hydrogen chloride – 2-propanol solution, ~1.25 M HCl (T), for GC derivatization, LiChropur
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Acetone, ≥99%, meets FCC analytical specifications
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Acetone, natural, ≥97%
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Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
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Acetone, analytical standard