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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 gas chromatography for the determination of residual organic solvents in silkworm excrement. METHODS: Headspace gas chromatography was used. The chromatographic column was DB-5MS quartz capillary column (30 m × 0.25 mm × 0.25 μm). The carrier gas was nitrogen and the flow rate was 0.6 ml · min -1 Sample temperature: 200 ℃; detector type and temperature: hydrogen flame ionization detector (FID) at 250 ℃; column temperature program: 40 ℃ for 10 min, and then at a rate of 5 ℃ · min ~ (-1) To 200 ° C for 5 min; headspace conditions: equilibrium temperature: 95 ° C; equilibration time: 30 min; transfer tube temperature: 110 ° C; injection loop temperature: 125 ° C. Results: Acetone, 2,3-dimethylpentane, 3-methylhexane, n-heptane, 2,2-dimethylhexane, paraxylene, metaxylene, The linear range of 6-trimethylpyridine was 101 ~ 3 034μg · ml -1, 100 ~ 2995μg · 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 and 104 ~ 3 130μg · ml -1, r values were above 0.992, the recovery rate was satisfactory, the blank solvent had no effect on the determination of the sample, and all 8 batches of samples were tested to meet the requirements . Conclusion: Headspace sampling gas chromatography for the determination of organic solvents in silkworm extract, the method is simple, the results are accurate.