GC法测定辣椒碱中环己烷、乙醇、乙酸乙酯残留量

Determination of cyclohexane,ethyl acetate and ethanol remained in capsicine by GC

目的建立气相色谱法测定辣椒碱中环己烷、乙醇、乙酸乙酯的残留量。方法色谱条件:检测器为氢火焰离子化检测器;固定相为6%氰丙基苯基-94%二甲基聚硅氧烷;色谱柱为石英毛细管柱30 m;载气柱流量2.0 mL·min-1;柱温为120℃维持10 min;气化室温度为200℃;检测器温度为250℃。结果在19.5～58.5μg·mL-1的范围内,环己烷的进样量与峰面积呈良好的线性关系,回归方程:Y=3.073 3X-0.158 4r,=0.998,平均回收率96.3%,RSD=3.5%。在25.0～75.0μg·mL-1的范围内,乙醇的进样量与峰面积呈良好的线性关系,回归方程:Y=1.620 8X-8.6r,=0.998,平均回收率99.4%,RSD为3.3%;在25.0～75.0μg·mL-1的范围内乙酸乙酯的进样量与峰面积呈良好的线性关系,回归方程:Y=1.387 2X-0.88r,=0.999,平均回收率97.4%,RSD为3.1%。结论本方法操作简单,准确、专属性强、重现性好,可作为辣椒碱中乙酸乙酯、环己烷、丙酮的残留量的测定方法。

Objective To establish a GC method for the determination of cyclohexane, ethyl acetate and ethanol remained in capsicine. Methods The chromatographic condition was as follows ： FID detector was used with 6% phenyl cyanide - 94% dime- thyl polysiloxane as stationary phase ; the capillary column was made of quartz （ 30 m ） and the flow rate was 2.0 mL · min^-1 with hydrogen as carrier gas;the column temperature was kept at 120 ℃ for 10 min,tbe injector temperature was 200 ℃ and the detec- tor temperature was 250 ℃. Results The linear range of cyclohexane was 19.5 ＋ 58.5 μg μ mL^-1 with the regression equation of Y = 3.073 3X - 0.158 4 （ r = 0.998 ） , the average recovery was 96.3 % with RSD of 3.5 % ;the linear range of ethanol was 25. 0 - 75.0 μg μ mL - 1 with the regression equation of Y = 1. 620 8X - 8.6 （ r = 0. 998 ） , the average recovery was 99.4% with RSD of 3.3% ;the linear range of ethyl acetate was 25.0- 75.0μg · mL^-1 with the regression equation of Y = 1. 387 2X - 0. 88 （ r = 0. 999） ,the average recovery of 97.4% and the RSD of 3.1%. Conclusion The method was simple, accurate, specific and reproducible, and it can be used for the determination of cyclohexane, ethanol and ethyl acetate remained in capsicine.