Chemical Faculty, Department of Chemical and Process Engineering, Gdansk University of Technology, G. Narutowicza St. 11/12, 80-233, Gdansk, Poland.
Anal Bioanal Chem. 2013 Jul;405(18):6095-103. doi: 10.1007/s00216-013-7038-3. Epub 2013 May 21.
The paper presents the results of investigations on new procedures of determination of selected cleaning additives in diesel fuel. Two procedures: one-step analysis using gas chromatography with flame ionization detection (GC-FID) or mass spectrometry (GC-MS) and a two-step procedure in which normal-phase high-performance liquid chromatography (NP-HPLC) was used for preliminary separation of the additives, were compared. The additive fraction was collected using either simple elution or eluent backflush. Final determinations were performed by GC-FID and GC-MS. The studies revealed that it was impossible to determine the investigated analytes by one-step procedures, i.e. by using solely HPLC or GC. On the other hand, the use of a two-step procedure ensures reproducible results of determinations, and the limits of quantitation are, depending on the method of fraction collection by HPLC, from 1.4-2.2 ppm (GC-MS in SIM mode) to 9.6-24.0 ppm (GC-FID). Precision and accuracy of the developed procedures are compared, and possible determination errors and shortcomings discussed.
本文介绍了对柴油中选定清洁添加剂的新测定程序的研究结果。比较了两种方法：一步分析法，使用火焰离子化检测（GC-FID）或质谱（GC-MS）的气相色谱法；两步法，其中正相高效液相色谱（NP-HPLC）用于添加剂的初步分离。添加剂部分采用简单洗脱或洗脱液反冲收集。最终测定采用 GC-FID 和 GC-MS。研究表明，仅使用 HPLC 或 GC 无法通过一步程序（即单一分析法）来测定所研究的分析物。另一方面，两步法的使用可确保测定结果的重现性，定量限取决于 HPLC 收集馏分的方法，从 1.4-2.2 ppm（GC-MS 在 SIM 模式下）到 9.6-24.0 ppm（GC-FID）。比较了所开发程序的精密度和准确度，并讨论了可能的测定误差和缺点。
