天津中医药2011,Vol.28Issue(6):506-509,4.
顶空进样气相色谱法测定脑脉通软胶囊中有机溶剂残留量
Determination of residual solvents in Naomaitong soft capsule by headspace GC
摘要
Abstract
[Objective] To establish the method for analysis on organic solvent residues in Naomaitong soft capsule in order to provide the basis for quality assessment. [Methods] GC instrument coupled with headspace sampler was used and taking 50% of the aqueous solution of dimethylformamide as the solvent. The column was DB-624 capillary column (75 mx0.530 mm,df=3.00 μm); FID detector temperature was 250 ℃; A nitrogen flow rate was set at 15 mL/min in a constant flow mode; Oven temperature program was used from 50 ℃(18 min) to 80 ℃ at a rate of 100 ℃/min ,then to 112 t at a rate of 2 t/min, next to 160 °C (10 min) at a rate of 100 t/min, finally to 200℃ (5 min) at a rate of 100 t/min; Gasification chamber temperature was 250 ℃. The headspace vials were balanced at 90 ℃ for 40 min, the injection time was 1 min. [Results] The residual solvents were not detected in Naomaitong soft capsule. A good linear behavior was found in the concentration ranging from 0 to 40 μg/mL. The LODs were 0.2~2.8 μg/ml,the precisions RSD were less than 5.6% (n=5). The average recoveries were in the range from 18.8% to 48.3%, with RSD of 0.5%~8.9% (n=5). The components of reference solution were stable within 24 h (RSD, 0.5%~8.9%,n=5). [Conclusion] The method is accurate, rapid and sensitive, so it can be used for controlling the organic residual solvents of Naomaitong.关键词
气相色谱法/有机溶剂残留量/大孔吸附树脂/脑脉通Key words
GC/ residues of organic solvent/ macroporous resin/Naomaitong分类
医药卫生引用本文复制引用
张在娟,逯获,崔丽霞,马莉,任晓文..顶空进样气相色谱法测定脑脉通软胶囊中有机溶剂残留量[J].天津中医药,2011,28(6):506-509,4.基金项目
国家重点基础研究发展计划项目(2010CB735602). (2010CB735602)