title: Optimization of experimental parameters in single-drop microextraction-gas chromatography-mass spectrometry for the determination of periodate by the Malaprade reaction, and its application to ethylene glycol.
abstract: The aim of present work was to optimize the experimental parameters in single drop microextraction under solution immersion (SDME) and headspace (HS-SDME) extraction modes for the determination of periodate using guaifenesine [3-(2'-methoxyphenoxy)-1,2-propane diol] and norephedrine (phenylpropanolamine) as new and alternative reagents for the Malaprade reaction. The reactions were complete within 5min resulting in the formation of 2-(2'-methoxyphenoxy)-acetaldehyde and benzaldehyde, respectively. SDME/HS-SDME of oxidation products with 2mul of anisole or 1mul of toluene, respectively, has permitted the determination of periodate at mugl(-1) concentration levels. The results indicated that HS-SDME (range 0.01-10mgl(-1), r(2)=0.9990; limit of detection 1.55mugl(-1)) was more sensitive than SDME (range 0.05-50mgl(-1), r(2)=0.9984; limit of detection 3.42mugl(-1)), and was inexpensive, rapid and convenient. Tolerance of excess of iodate has permitted the application of this method in the determination of ethylene glycol in motor oil; the average recovery on spiked sample was 98.6% with R.S.D. of 4.2%.
authors.affiliation: Department of Chemistry, Rani Durgavati University, Jabalpur 482001, Madhya Pradesh, India.
authors.forename: Manju
authors.initials: M
authors.lastname: Gupta
authors.forename: Archana
authors.initials: A
authors.lastname: Jain
authors.forename: Krishna K
authors.initials: KK
authors.lastname: Verma