毛细管柱气相色谱法测定甲酚及甲酚皂溶液的含量  被引量:3

Capillary GC determination of cresol and saponated cresol solution

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作  者:于大海[1] 苏佳妍[2] 李庆民[1] 

机构地区:[1]辽宁省食品药品检验所,沈阳110023 [2]中国医科大学第一临床医院药剂科,沈阳110001

出  处:《药物分析杂志》2009年第11期1867-1869,共3页Chinese Journal of Pharmaceutical Analysis

摘  要:目的:改进现有甲酚及甲酚皂溶液含量测定中各组分均不能完全得以分离的缺陷,建立一个新的气相色谱方法。方法:采用毛细管柱气相色谱法,安捷伦6890型气相色谱仪;安捷伦DB-225毛细管柱,(50%氰丙基苯基)二甲基聚硅氧烷为固定液,长30m、内径0.32mm、膜厚0.25μm。程序升温110℃(31min)20℃.min-1150℃(10min),载气:99.99%氮气,流速1mm.min-1;采用分流进样,进样量1μL。结果:采用毛细管柱气相色谱法能较大地提高组分之间的分离度。甲酚中各组分的线性关系为,邻甲酚:Y=3.77X-0.0087(y=0.9998);对甲酚:Y=3.67X-0.0011(y=0.9996);间甲酚:Y=3.58X-0.0068(y=0.9997)。平均回收率为98.99%,RSD=0.95%(n=9)。结论:本法准确,专属性好,可用作控制甲酚及甲酚皂溶液质量的方法。Objective: Set up a new gas chromatographic method to improve the existing Cresol and saponated cresol solution determination of each component which can not be completely separated from the defect,. Methods: Using capillary gas chromatography, Agilent 6890 gas chromatograph; Agilent DB-225 capillary column (50% n-propyl cyanide phenyl) dimethyl polysiloxane as stationary phase, long 30m, internal diameter of 0.32mm, film thickness 0.25μm. The column temperature was 110℃ to 150℃ and rose by the program: 110℃(31min)20℃·min^-1→ 150℃(10min), carrier gas: 99.99% N2 ,flow rate of 1mm · min^-1; the use of split injection, injection volume of 1μL. Results: Using capillary gas chromatography to enhance the separation between the components, Each component of the linear relationship was O-cresol: Y=3.77X-0.0087(γ=0.9998);P-cresol:Y=3.67X-0.0011(γ=0.9996);M-cresol:Y=3.58X-0.0068(γ=0.9997).The average recovery was 98.99 %,RSD=0.95%(n=9). Conclusion: The method developed is accurate and sensitive which can be applied to determination of Cresol and saponated cresol solution.

关 键 词:甲酚 甲酚皂 毛细管柱气相色谱法 

分 类 号:R917[医药卫生—药物分析学]

 

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