GC法测定三七三醇皂苷中8种大孔吸附树脂的残留物  

Determination of eight kinds of macroporous resin residues in panaxatriol saponins by headspace GC

作　　者：马茹君[1,2] 王莉[2] 杨华蓉[2] 高星[2] 刘峰 

机构地区：[1]四川大学华西药学院,四川成都610041 [2]成都华神集团股份有限公司制药厂,四川成都610225 [3]四川省食品药品检验检测院,四川成都610075

出　　处：《华西药学杂志》2016年第2期202-205,共4页West China Journal of Pharmaceutical Sciences

基　　金：国家发改委项目(发改办高技2011-51号);成都高新区生物医药研发及产业化项目:三七通舒胶囊国际化(欧盟)药品注册合作研究

摘　　要：目的采用顶空气相色谱法同时测定三七三醇皂苷中8种大孔吸附树脂的残留物。方法色谱柱为Agilent innowax柱（30 m×0.32 mm,0.5μm）,二甲亚砜为溶解介质,FID检测器,进样口温度140℃,检测器温度250℃,高纯氮作载气,程序升温（50℃保持20 min,再以6℃·min^-1升至165℃,保持20 min）。结果各组分在所考察的浓度范围内均具有良好的线性,r为0.9903~0.9998,RSD为1.13%~6.99%,正己烷、环己烷、1,1,1-三氯乙烷、苯、甲苯、邻二甲苯、间二甲苯、对二甲苯的最低检出浓度分别为0.1389、0.3056、6.4980、0.5528、0.8282、1.9962、1.9500、2.6900 mg·kg^-1。结论所用方法快速、灵敏、准确,适用于三七三醇皂苷中大孔吸附树脂残留物的测定。OBJECTIVE To establish a headspace GC method for simultaneous determination of the eight kinds of macroporous resin residues in panaxatriol saponins. METHODS Headspace GC with Agilent innowax column（ 30 m × 0. 32 mm,0. 5 μm）,the solvent medium was dimethyl sulfoxide and the detector was FTD. The injector temperature was 140 ℃ with the detector temperature of 250 ℃,and the carrier gas of high- purity nitrogen. The column temperature was changed according to the program： initial temperature was kept at 50 ℃ for 20 min,then raised to 165 ℃ at the rate of 6 ℃·min^-1,and totally maintained for 20 min. RESULTS The results showed good linearity（ 0. 9903- 0. 9998）,and RSD of precision were in the range of 1. 13%- 6. 99%. The minimum detection concentrations of n- hexane,cyclohexane,1,1,1- trichloroethane,benzene,methylbenzene,o- xylene,m- xylene and p- xylene was 0. 1389,0. 3056,6. 4980,0. 5528,0. 8282,1. 9962,1. 9500,2. 6900 mg·kg^-1,respectively. CONCLUSION The method is simple,sensitive and accurate,and suitable for the determination of macroporous resin residues in panaxatriol saponins.

关 键 词：顶空气相色谱法 三七三醇皂苷 大孔吸附树脂 残留物 安全性 检测 

分 类 号：R917[医药卫生—药物分析学]