美缝剂中壬基酚含量测定

Determination of Nonylphenol Content in Sealant

利用气相色谱质谱联用仪进行定性定量分析美缝剂产品中壬基酚含量。以乙酸丁酯为溶剂,通过超声萃取样品。采用DB-5毛细管柱(30m×320μm×0.25μm)为分离柱。进样口温度设定为300℃;采用程序升温,起始温度为70℃保持2min,以10℃/min升至280℃保持2min。质谱采用SIM扫描,监控离子为107 121 135,在该色谱条件下美缝剂产品中壬基酚能与杂质分离,线性相关系数0.9980,检出限为0.1mg/mL。前处理采用乙酸丁酯超声提取,样品加标回收率为97.8%~98.8%。经验证该方法适合用于美缝剂产品中壬基酚含量检验。

The content of nonylphenol in sealant products was quantitatively and qualitatively determined by gas chromatography-mass spectrometry.The samples were extracted by ultrasonic with butyl acetate as solvent.A DB-5 capillary column(30m×320μm×0.25μm)was used as the separation column.The inlet temperature was set at 300℃.Programmed heating was adopted,with the initial temperature of 70℃held for 2min.and the temperature was increased to 280℃held for 2min at 10℃/min.The mass spectrum adopts SIM scanning,and the monitoring ions are 107121135.Under this chromatogram condition,nonylphenol in the suture product can be separated from impurities.The linear correlation coefficient is 0.9980,and the detection limit is 0.1mg/mL.Pre-treatment was performed by ultrasonic extraction of butyl acetate.The recoveries are 97.8%-98.8%.It is proved that this method is suitable for the determination of nonylphenol content in sealant products.