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Determination of residual solvents and reagents in X-ray contrast media by automatic static headspace capillary gas chromatography

✍ Scribed by Evje, Dag M. ;Figenschou, Erik ;Langseth-Manrique, Karina


Publisher
John Wiley and Sons
Year
1990
Tongue
English
Weight
412 KB
Volume
13
Category
Article
ISSN
0935-6304

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✦ Synopsis


Abstract

A specific, sensitive, and simple method for the quantitation of residual methanol, 2‐propanol, 2‐butanol, 2‐methoxy‐1‐ethanol, 1‐chloro‐3‐methoxy‐2‐propanol, 3‐chloro‐2‐methoxy‐1‐propanol, and 1,3‐dimethoxy‐2‐propanol in two non‐ionic X‐ray contrast media, has been developed. The headspace of a 25 % w/V aqueous solution of contrast media, obtained at 90–110°C in 15 min, was injected onto a capillary column coated with cyanopropyl, phenyl, dimethylpolysiloxane polymer. The internal standards used were 2‐pentanol and 3‐methoxy‐1‐butanol. The limits of detection were below 5 μg/g. The repeatability of the method at 50 μg/g of each solvent was below 5 %; and at 100 μg/g of the methoxypropanol compounds and 2‐methoxy‐1‐ethanol, below 10 % (RSD, N = 5).


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## Abstract Static headspace (HS) sampling has been commonly used to test for volatile organic chemicals, usually referred to as residual solvents (RS) in pharmaceuticals. If the sample is not soluble in water, organic solvents are used. However, these seriously reduce the sensitivity in the determ