顶空气相色谱法检测石茶感冒胶囊中的有机溶剂残留 |
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引用本文: | 何雷,;崔涛,;夏伟军,;丁中涛.顶空气相色谱法检测石茶感冒胶囊中的有机溶剂残留[J].国外医药(植物药分册),2009(6):347-349. |
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作者姓名: | 何雷 ;崔涛 ;夏伟军 ;丁中涛 |
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作者单位: | [1]云南省药物研究所新药筛选研究中心,云南昆明650111; [2]云南大学化学科学与工程学院,云南昆明650091 |
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基金项目: | 云南省科技厅省科研院所技术开发研究专项(2003KFZX-28) |
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摘 要: | 目的建立石茶感冒胶囊中可能残留的7种有机溶剂(正己烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、二乙烯苯)的检测方法。方法采用顶空气相色谱法,色谱柱为Agilent HP—INNOWAX毛细管柱(30m×1.0mm,0.53μm),载气为高纯氮气;项空温度为70℃,顶空时间30min;柱温自30℃恒定5min,以10℃/min升温速率升至200℃,恒定5min;氢火焰离子检测器(FID),温度为250℃。结果7种有机溶剂残留物在所考察的浓度范围内线性关系良好(r=0.9994~0.9998),精密度RSD均小于5.0%,被测组分的平均回收率在99.16%~102.0%之间。结论该方法操作简便、快速、准确度高,可用于检测石茶感冒胶囊中的有机溶剂残留物。
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关 键 词: | 石茶感冒胶囊 顶空气相色谱 有机溶剂残留 残留物测定 |
Determination of residual organic solvents in Shicha Ganmao Capsule by gas chromatography with headspace sampling |
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Institution: | HE Lei, CUI Tao, XIA Wei-jun, DING Zhong-tao (1. Natural Medicine Chemical Research Section, Yunnan Institute of Materia Medica, Kunming 650111, China; 2. School of Chemical Science and Technology, Yunnan University, Kunming 650091, China) |
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Abstract: | Objective To establish a method for determination of the seven residual organic solvents (nhexane, benzene, toluene, o-dimethylbenzene, p-dimethylbenzene, styrene and divinyl benzene) in Shicha Ganmao Capsule. Methods Gas chromatography with headspace sampling was applied to the study. Agilent HP-INNOWAX silica capillary column was 30 m × 1.0 mm, 0.53 μm. The initial temperature was kept at 30 ℃ for 5 min, then the temperature was raised to 200 ℃ at the rate of 10 ℃/min and subsequently sustained for 5 min. FID detector temperature was 250 ℃. The vial temperature was 70 ℃, and the vial time was 30 min. Results There was a good linearity in the experimental concentration (r= 0. 999 4- 0. 999 8). The RSD was all less than 5.0%. The average recovery rates were in the range of 99.16%- 102.0%. Conclusion The analytical method is simple, accurate and sensitive. |
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Keywords: | Shicha Ganmao Capsule gas chromatography with headspace sampling residual organic solvent determination of residues |
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