Optimization of experimental parameters in single-drop microextraction–gas chromatography–mass spectrometry for the determination of periodate by the Malaprade reaction, and its applicat
- 作者：Manju Gupta ; Archana Jain ; Krishna K. Verma
- 关键词：Single-drop microextraction ; Immersion ; Headspace ; Periodate ; Ethylene glycol ; GC– ; MS
- 刊名：Talanta
- 出版年：2007
- 期刊代码：106_00399140
- 类别：ch
- 出版时间：28 February 2007
- 卷：71
- 期：3
- 页码：1039-1046
- 文件大小：595 K
摘要
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 5 min resulting in the formation of 2-(2′-methoxyphenoxy)-acetaldehyde and benzaldehyde, respectively. SDME/HS-SDME of oxidation products with 2 μl of anisole or 1 μl of toluene, respectively, has permitted the determination of periodate at μg l−1 concentration levels. The results indicated that HS-SDME (range 0.01–10 mg l−1, r2 = 0.9990; limit of detection 1.55 μg l−1) was more sensitive than SDME (range 0.05–50 mg l−1, r2 = 0.9984; limit of detection 3.42 μg l−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%.