Centre for Analytical Science, Department of Chemistry, Loughborough University, Loughborough, LE11 3TU, UK.
Rapid Commun Mass Spectrom. 2013 Nov 15;27(21):2420-4. doi: 10.1002/rcm.6690.
Chemical additives are incorporated into commercial lubricant oils to modify the physical and chemical properties of the lubricant. The quantitative analysis of additives in oil-based lubricants deposited on a surface without extraction of the sample from the surface presents a challenge. The potential of desorption electrospray ionization mass spectrometry (DESI-MS) for the quantitative surface analysis of an oil additive in a complex oil lubricant matrix without sample extraction has been evaluated.
The quantitative surface analysis of the antioxidant additive octyl (4-hydroxy-3,5-di-tert-butylphenyl)propionate in an oil lubricant matrix was carried out by DESI-MS in the presence of 2-(pentyloxy)ethyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate as an internal standard. A quadrupole/time-of-flight mass spectrometer fitted with an in-house modified ion source enabling non-proximal DESI-MS was used for the analyses.
An eight-point calibration curve ranging from 1 to 80 µg/spot of octyl (4-hydroxy-3,5-di-tert-butylphenyl)propionate in an oil lubricant matrix and in the presence of the internal standard was used to determine the quantitative response of the DESI-MS method. The sensitivity and repeatability of the technique were assessed by conducting replicate analyses at each concentration. The limit of detection was determined to be 11 ng/mm(2) additive on spot with relative standard deviations in the range 3-14%.
The application of DESI-MS to the direct, quantitative surface analysis of a commercial lubricant additive in a native oil lubricant matrix is demonstrated.
化学添加剂被掺入商业润滑油中,以改变润滑剂的物理和化学性质。在不从表面提取样品的情况下,对沉积在表面上的基于油的润滑剂中的添加剂进行定量分析是一项挑战。本文评估了在无需提取样品的情况下,解吸电喷雾电离质谱(DESI-MS)在复杂油润滑剂基质中对油添加剂进行定量表面分析的潜力。
通过 DESI-MS 对油润滑剂基质中的抗氧化添加剂辛基(4-羟基-3,5-二叔丁基苯基)丙酸进行定量表面分析,同时使用 2-(戊氧基)乙基 3-(3,5-二叔丁基-4-羟基苯基)丙酸作为内标。使用配备有内部改装的离子源以实现非近程 DESI-MS 的四极杆/飞行时间质谱仪进行分析。
使用 1 至 80 µg/spot 的辛基(4-羟基-3,5-二叔丁基苯基)丙酸在油润滑剂基质中的八点校准曲线和内标来确定 DESI-MS 方法的定量响应。通过在每个浓度下进行重复分析来评估该技术的灵敏度和重复性。检测限确定为 11 ng/mm2 的添加剂斑点,相对标准偏差在 3-14%范围内。
证明了 DESI-MS 可直接对天然油润滑剂基质中的商业润滑剂添加剂进行定量表面分析。