气相色谱法测定羟苯丁酯中8种有机溶剂的残留量

Determination of residues of 8 organic solvents in butylparaben by GC

目的建立同时测定羟苯丁酯中甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇和叔丁醇8种有机溶剂残留量的气相色谱法。方法采用DB-624毛细管柱(0.32 mm×30 m,1.8μm);FID检测器;进样口温度为200℃,检测器温度为250℃;载气为高纯氮气,载气流速为2 mL·min^-1;升温程序,起始温度45℃,保持2 min,以5℃·min^-1升温至65℃保持5 min,再以40℃·min^-1升温至200℃保持2 min。结果羟苯丁酯中8种残留溶剂在各自线性浓度范围内与峰面积线性关系良好(r均>0.999);平均回收率在104.0%~105.2%。结论本方法操作简单、准确度高、重现性好,可用于羟苯丁酯中8种有机溶剂残留量的测定。

Objective To establish GC method to simultaneously determine the residues of 8 organic solvents(methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol and tert-butanol) in butylparaben. Methods The determination was performed on DB-624 capillary column(30 m×0.53 mm, 3.0 μm) with temperature programming by FID. The inlet temperature was 200 ℃ and the detector temperature was 250 ℃. The carrier gas was high purity nitrogen, and the carrier gas flow rate was 2 mL·min^-1. The column temperature started at 45 ℃ for 2 min, and then at 5 ℃·min^-1 to 65 ℃ for 5 min, followed by 40 ℃·min^-1 to 200 ℃ for 2 min. Results The 8 residual solvents in butylparaben had a good linear relationship in their concentration ranges(r > 0.999). The average recovery was 104.0%-105.2%. Conclusion The method is simple, accurate and reproducible and can be used to determine the residues of 8 organic solvents in butylparaben.