Kennan J J, Breen L L, Lane T H, Taylor R B
Dow Corning Corporation, Midland, Michigan 48686-0994, USA.
Anal Chem. 1999 Aug 1;71(15):3054-60. doi: 10.1021/ac990157d.
Methods for analyzing for silicon and silicone in biological matrixes were developed. A silicone-specific technique involved microwave digestion of samples in acid solution to rapidly break down the biological matrix while hydrolyzing silicones to monomeric species. The resulting monomeric silanol species were then capped with trimethylsilyl groups, extracted into hexamethyldisiloxane, and analyzed by gas chromatography. In serum, positive identification of silicone species with detection limits below 0.5 microgram of Si/mL are possible with this technique. The technique is compared with a silicone-specific technique, 29Si NMR, and a non-silicone-specific technique, ICP-AES. 29Si NMR was far less sensitive, with a detection limit of only 64 micrograms of Si/mL in serum when analyzing for one compound with a single sharp resonance. Inductively coupled plasma-atomic emission spectroscopy (ICP-AES) has potentially lower detection limits, but the technique is not silicone-specific and suffers from species-dependent responses.
开发了用于分析生物基质中硅和硅氧烷的方法。一种针对硅氧烷的技术包括在酸性溶液中对样品进行微波消解,以快速分解生物基质,同时将硅氧烷水解为单体形式。然后将生成的单体硅醇物种用三甲基硅烷基封端,萃取到六甲基二硅氧烷中,并通过气相色谱进行分析。使用该技术可以在血清中对硅氧烷物种进行阳性鉴定,检测限低于0.5微克硅/毫升。将该技术与一种针对硅氧烷的技术(29Si NMR)和一种非针对硅氧烷的技术(电感耦合等离子体原子发射光谱法,ICP-AES)进行了比较。29Si NMR的灵敏度要低得多,在分析具有单个尖锐共振的一种化合物时,血清中的检测限仅为64微克硅/毫升。电感耦合等离子体原子发射光谱法(ICP-AES)的检测限可能更低,但该技术并非针对硅氧烷,且存在物种依赖性响应。