赤芍提取物有机溶剂残留检测研究

A Study on Determination of Residual Solvents in Paeoniae Extract

目的:建立赤芍提取物中2种有机溶剂残留量的检测方法。方法:采用顶空气相色谱法,以正丙醇为内标物对乙醇、正丁醇进行检测。以FFAP毛细管柱(30m×0.53mm,1μm)为色谱柱,柱温为60℃,载气为氮气,柱前压20kPa,进样口温度为220℃,FID检测器,检测器温度为250℃,空气流速500ml/min,氢气流速50ml/min。结果:乙醇、正丁醇分别在2.5～240mg/L(r=0.9996),0.5～48mg/L(r=0.9999)的浓度内呈良好的线性关系;平均回收率分别为99.95%、99.93%(RSD=3.5、3.2,n=9)。结论:顶空气相色谱法简便、快速、重现性好,适用于赤芍提取物中有机溶剂残留量的检测。

Objective： To establish a method for determination of two residual solvents in Paeoniae extract. Methods： The residual solvents （ethanol and n-butanol） were quantitatively determined by using headspace gas chromatography （GC） with n-propanol as internal standard. A FFAP capillary column（30 m ×0. 53 mm,1 μm）was used at 60℃. Nitrogen was used as carrier gas. The column inlet pressure was 20 kPa. The temperature at the injection port and the FID detector were 220 ℃ and 250℃, respectively. The flow rate of air and hydrogen were 500 ml/min and 50 ml/min. Results： Ethanol and n-butanol showed a good linear relation at the range of 2. 5 - 240 mg/L（ r = 0. 999 6） and 0. 5 -48 mg/L（r =0. 999 9） , with mean recovery rates of 99.95% and 99.93% （RSD =3.5,3.2,n = 9）, respectively. Conclusion： The method is simple, rapid and reproducible. It can be used for the determination of residual solvents in Paeoniae extract.