Garrido-López Alvaro, Esquiu Vanesa, Tena María Teresa
Chemistry Department, University of La Rioja, C/ Madre de Dios 51, E-26006 Logroño (La Rioja), Spain.
J Chromatogr A. 2007 May 25;1150(1-2):178-82. doi: 10.1016/j.chroma.2006.11.090. Epub 2006 Dec 11.
Polymers require the use of some slip agents, such as oleamide and erucamide, in order to reduce their friction coefficient and to make films easier to handle. In this communication, three analytical methods consisting in pressurized liquid extraction (PLE) and gas chromatography (GC) are used to determine oleamide and erucamide in polyethylene films. The sample was extracted with pure isopropanol (two times) at 105 degrees C for 16 min. Then, the liquid extract containing oleamide and erucamide was analyzed by GC and three different detection systems: flame ionization detector (FID), thermoionic selective detector (TSD) and ion-trap mass spectrometry detector (MSD). Oleamide and erucamide were separated using a 30 m x 0.25 mm (I.D.) 5% phenyl-95% dimethyl-polysiloxane capillary column in 12 min. The chromatographic methods were characterized and compared in terms of repeatability, linearity and sensitivity. The GC-FID and GC-TSD methods were linear up to about 60 microg ml(-1), whereas the linear range for the GC-MSD method was shorter, from 20.5 to 42 microg ml(-1). LODs identified with GC-MSD were two times higher than those identified with the other two methods. Repeatability values (expressed as relative standard deviation) of less than 2.5% were found for FID and TSD but they were above 10% for MSD. Finally, each method was applied to determine the content of erucamide and oleamide in several polyethylene films and the results obtained were compared with those obtained from the nitrogen content measured by pyrolysis and gas-phase chemiluminescence. No significant differences were observed between the results of the methods.
聚合物需要使用一些爽滑剂,如油酰胺和芥酸酰胺,以降低其摩擦系数并使薄膜更易于处理。在本通讯中,采用了三种分析方法,包括加压液体萃取(PLE)和气相色谱(GC)来测定聚乙烯薄膜中的油酰胺和芥酸酰胺。样品在105℃下用纯异丙醇萃取(两次)16分钟。然后,通过GC和三种不同的检测系统对含有油酰胺和芥酸酰胺的液体提取物进行分析:火焰离子化检测器(FID)、热离子选择性检测器(TSD)和离子阱质谱检测器(MSD)。使用30 m×0.25 mm(内径)5%苯基-95%二甲基聚硅氧烷毛细管柱在12分钟内分离出油酰胺和芥酸酰胺。从重复性、线性和灵敏度方面对色谱方法进行了表征和比较。GC-FID和GC-TSD方法在高达约60μg ml-1时呈线性,而GC-MSD方法的线性范围较短,为20.5至42μg ml-1。GC-MSD确定的检测限比其他两种方法确定的检测限高两倍。FID和TSD的重复性值(以相对标准偏差表示)小于2.5%,但MSD的重复性值高于10%。最后,将每种方法应用于测定几种聚乙烯薄膜中芥酸酰胺和油酰胺的含量,并将所得结果与通过热解和气相化学发光法测定的氮含量所得结果进行比较。各方法的结果之间未观察到显著差异。