新型碳纳米管固相微萃取-气相色谱法测定义齿基托树脂中游离甲基丙烯酸酯类

Determination of free methacrylic acid in denture base resin by HS-SPMS-GC using a novel carbon nanotube coated fiber

采用顶空进样-固相微萃取-气相色谱法,以溶胶-凝胶技术涂渍碳纳米管新型固相微萃取探头(CNT-101),对国产自凝义齿基托树脂和进口自凝义齿基托树脂中的痕量游离甲基丙烯酸酯类进行了检测。实验中,对解吸温度、解吸时间、萃取温度、萃取时间、离子强度、搅拌速度等条件进行了优化。在样品用量8mL、解吸温度300℃、解吸时间1min、萃取温度室温、萃取时间30min、加入饱和氯化钠、搅拌速度1200r/min的条件下进行了气相色谱法测定,3种甲基丙烯酸酯(甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯)峰面积的相对标准偏差(RSD,n=5)<5%,在20～2000μg/L浓度范围内呈良好的线性关系(r>0.99),方法检测限为4.7～48.3ng/L。该方法集萃取、富集、进样于一体,简便、灵敏,检测限低,适用于义齿基托树脂中微量游离甲基丙烯酸酯类的检测。

Three trace free methacrylates,in self-clotting denture base resins were determined by head space-solid phase microextraction-gas chromatography（HS-SPMS-GC） using a SPME fiber coated with carbon nanotube by sol-gel technique.The operational conditions of SPME were optimized：thermal desorption temperature,300℃;thermal desorption time,1 min;Stirring rate,1200r/min;extraction time,30min;extraction temperature,room temperature;ion intensity,saturation.Under these conditons,when the sample volume is 8mL,the RSDs of peak areas were 〈5%（n=5）,for three free methacrylates the linear range were 20～2000μL（r=0.99）,and the detection limits were 4.7～48.3ng/L.The method integates sampling,separation,extration and injection into one single step,and it is simple,fast,sensitive and suitable for trace amount detection.