利用HS-GC/MS和响应面法分析纸中溶剂残留的方法研究

本研究以N,N-二甲基乙酰胺为稀释剂,使用顶空-气相色谱质谱联用分析法（HS-GC/MS）测定了纸质包装材料中常见的8种有机溶剂的残留。采用HP-5MS色谱柱分离有机溶剂,He气流速为1ml/min;进样口温度250℃;升温程序为初始温度35℃,保持3min,以10℃/min速率升温至100℃,保持2min,共11.5min可以将8种有机溶剂分离开来。运用响应面法优化前处理温度和时间,发现前处理温度对峰面积影响显著,而前处理时间影响较不显著;最佳前处理温度为100℃,时间40min。该实验条件下,计算回归方程和相关系数,根据信噪比（S/N）为3,确定检出限。结果得到：8种残留溶剂的线性范围为0.330-7.956mg/m~2,线性相关系数为0.9952-0.9997,检出限为0·01-0.38mg/m^2;加标回收率为99%-114.8%,相对标准偏差RSD（n=5）为0.916%-1.455%。

Study on Detecting Organic Solvents Residue in Paper Using HS-GC/MS and Response Surface Method

Abstract In this study, HS - GC/MS was used to determine 8 kinds of residual solvents in paper with N, N - Dimethylacet- amide as the diluent. 8 kinds of residual solvents can be effectively segregated by HP -SMS chromatographic column in the conditions （the flow velocity of He of lml/min, inlet temperature of 250 ℃ keeping 2 rain in the initial temperature of 35℃, then heating to 100 ℃ at 10 ℃/rain rate to keep 2min, the total time of 11.5min）. Response surface method was used to optimize pretreatment temperature and time. The experimented results found that pretreatment temperature change was significant for peak area, pretreatment time was less influence, the optimal pretreatment temperature of 100℃ and time of 40min. On optimized condition, regression equation and correlation coefficient were calculated, and detection limit was determined according to S/N of 3. The results showed that the range of linearity is well from 0.330 -7. 956mg/mz, linear correlation coefficient is 0.9952 -0.9997 and detection limit is 0.01 -0.38mg/m2. The average recovery is 99%- 114.8% and the RSD of precision （ n = 5） is 0.916%- 1. 455%.