气相色谱法测定蚕砂提取物中有机溶剂残留量  

Determination of Residual Solvents in Faeces Bombycis Extract by GC

作　　者：周伟 邹瑞 

机构地区：[1]湖北省食品药品监督检验研究院,武汉430075

出　　处：《中国药师》2016年第6期1211-1214,共4页China Pharmacist

摘　　要：目的:建立测定蚕砂提取物中有机溶剂残留量的气相色谱法。方法:采用顶空进样气相色谱法,色谱柱:DB-5MS石英毛细管色谱柱(30 m×0.25 mm×0.25μm);载气:氮气;流速:0.6 ml·min^(-1);进样口温度:200℃;检测器类型及温度:氢焰离子化检测器(FID),250℃;柱升温程序:40℃保持10 min,然后以5℃·min^(-1)的速度升至200℃,保持5 min;顶空条件:平衡温度:95℃;平衡时间:30 min;传输管温度:110℃;进样环温度:125℃。结果:丙酮,2,3-二甲基戊烷,3-甲基己烷,正庚烷,2,2-二甲基己烷,对二甲苯,间二甲苯,邻二甲苯,2,4,6-三甲基吡啶的线性范围分别为:101~3 034μg·ml^(-1),100~2 995μg·ml^(-1),107~3 197μg·ml^(-1),101~3 019μg·ml^(-1),99~2 962μg·ml^(-1),45~1 358μg·ml^(-1),44~1 325μg·ml^(-1),47~1 411μg·ml^(-1)和104~3 130μg·ml^(-1),r值均在0.992以上,回收率符合要求,空白溶剂对样品的测定没有影响,8批样品检验均符合限度要求。结论:顶空进样气相色谱法测定蚕砂提取物中有机溶剂,方法简单,结果准确。Objective： To establish a method for the determination of solvent residues in faeces bombycis extract by GC. Meth- otis： A GC-headspace injection method was adopted to detect the residual organic solvents in the extract of faeces bombycis. A DB- 5MS （30 m x0.25 mmx 0.25 μm） quartz capillary column was used as the chromatographic column;nitrogen was used as the carrier gas at a flow rate of 0.6 ml·min-1 ;the injector temperature was 200℃ ;the detector was a flame ionization detector （FID） with the temperature of 250℃ ; the temperature program included two phases ： the initial temperature was set at 40℃ for 10 min, and then risen to 200℃ at a rate of 5 ℃·min-1 and maintained for 5 min;the equilibrium temperature of headspace was 95℃ ;the equilibrium time was 30 min;the capillary temperature was 110℃ ; the injection ring temperature was 125℃. Results： The linear range of acetone, 2, 3-dimethylpentane, 3-methylhexane, heptane, 2,2-dimethylhexane, p-xylene, m-xylene, O-xylene and 2,4,6-collidine was 101-3 034μg·ml-1 , 100-2 995μg·ml-1 , 107-3 197μg·ml-1 , 101-3 019 μg·ml-1 , 99-2 962 μg·ml-1 , 45-1 358 μg·ml-1 , 44-1 325μg·ml-1 , 47-1 411μg·ml-1 and 104-3 130 μg·ml-1, respectively, and the average r was all above 0.992. The recovery of the method met the requirement, and the blank solvent showed no interference. Eight samples were all accordance with the requirements after the examination. Conclusion： The headspace injection method for the determination of residual organic solvents in the extract of faeces bombycis is simple and reliable.

关 键 词：顶空选样气相色谱法 有机溶剂残留 蚕砂提取物 

分 类 号：R927.1[医药卫生—药学]