Wejnerowska Grazyna, Karczmarek Anna, Gaca Jerzy
Department of Chemistry and Environmental Protection, Faculty of Chemical Technology and Engineering, University of Technology and Agriculture in Bydgoszcz, Seminaryjna 3 St., 85-326 Bydgoszcz, Poland.
J Chromatogr A. 2007 May 25;1150(1-2):173-7. doi: 10.1016/j.chroma.2006.10.030. Epub 2006 Oct 30.
A new method for determination of fluoride in toothpaste employing the headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/flame ionization detection (GC/FID) has been proposed. It is a development of the method for determination of fluoride using trimethylchlorosilane (TMCS) as the derivatization reagent to form trimethylfluorosilane (TMFS), with the liquid/liquid extraction (LLE) step replaced by HS-SPME. To introduce the latter, it was necessary to determine the conditions of the reaction and to optimize the two stages of the SPME procedure: extraction and desorption. The parameters of the SPME analysis using carboxen/polydimethylsiloxane (CAR/PDMS) fiber were defined and compared with the corresponding ones for the LLE method, used as a reference. Also, these two methods were compared with respect to their linearity, precision, and accuracy. Results from toothpaste analyses using these two methods were highly correlated, indicating the potential to use the SPME extraction as an inexpensive and solventfree alternative to the LLE method.
提出了一种采用顶空固相微萃取（HS-SPME）结合气相色谱/火焰离子化检测（GC/FID）测定牙膏中氟化物的新方法。它是使用三甲基氯硅烷（TMCS）作为衍生化试剂形成三甲基氟硅烷（TMFS）来测定氟化物方法的改进，其中液液萃取（LLE）步骤被HS-SPME所取代。为引入后者，有必要确定反应条件并优化SPME程序的两个阶段：萃取和解吸。定义了使用碳分子筛/聚二甲基硅氧烷（CAR/PDMS）纤维的SPME分析参数，并与用作参考的LLE方法的相应参数进行比较。此外，还比较了这两种方法的线性、精密度和准确度。使用这两种方法进行牙膏分析的结果高度相关，表明使用SPME萃取作为LLE方法的一种廉价且无溶剂替代方法的潜力。
