Kumooka Y
National Research Institute of Police Science, 6-3-1, Kashiwanoha, Kashiwa, Chiba 277-0882, Japan.
Forensic Sci Int. 2008 Apr 7;176(2-3):111-20. doi: 10.1016/j.forsciint.2007.07.009. Epub 2007 Aug 28.
The optimum method for analyzing glyceryl rosinate by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) was studied. The performances of dithranol, anthracene, and 2,5-dihydroxybenzoic acid, pyrene, trans,trans-1,4-diphenyl-1,3-butadiene, 9-nitroanthracene, indole-3-acrylic acid and retinoic acid as a matrix agent, and those of sodium trifluoroacetate (NaTFA) and silver trifluoroacetate (AgTFA) as a cationization agent were measured. Dithranol showed higher signal to noise ratio and lower base-line, and AgTFA showed better performance than NaTFA. In this study, however, NaTFA was chosen since the ester peaks with high signal to noise ratios were observed, and the spectra of sodium-cationized molecules are simpler than those of silver-cationized molecules. Rosin esters and modified rosin esters in 22 rubber-based pressure sensitive adhesives and a paper-cement were analyzed. Glyceryl rosinate, glyceryl disproportionated rosinate, pentaerythrityl rosinate and pentaerythrityl hydrogenated rosinate were easily detected despite the fact that rubber-based adhesives are complex mixtures of elastomers, tackifiers, antioxidants and other additives. The detection limit of this method was studied and 2% of glyceryl rosinate in a rubber-based pressure sensitive adhesive was detected. It has been proved that MALDI-TOF-MS is a useful analytical method to analyze rosin and modified rosin esters in adhesives.
研究了用基质辅助激光解吸/电离飞行时间质谱法(MALDI-TOF-MS)分析松香甘油酯的最佳方法。测定了作为基质剂的蒽林、蒽、2,5-二羟基苯甲酸、芘、反式,反式-1,4-二苯基-1,3-丁二烯、9-硝基蒽、吲哚-3-丙烯酸和视黄酸的性能,以及作为阳离子化剂的三氟乙酸钠(NaTFA)和三氟乙酸银(AgTFA)的性能。蒽林显示出较高的信噪比和较低的基线,并且AgTFA的性能优于NaTFA。然而,在本研究中选择了NaTFA,因为观察到具有高信噪比的酯峰,并且钠阳离子化分子的光谱比银阳离子化分子的光谱更简单。分析了22种橡胶基压敏胶和一种纸胶中的松香酯和改性松香酯。尽管橡胶基胶粘剂是弹性体、增粘剂、抗氧化剂和其他添加剂的复杂混合物,但仍能轻松检测到松香甘油酯、歧化松香甘油酯、季戊四醇松香酯和季戊四醇氢化松香酯。研究了该方法的检测限,并检测到橡胶基压敏胶中2%的松香甘油酯。事实证明,MALDI-TOF-MS是分析胶粘剂中松香和改性松香酯的一种有用的分析方法。