聚酰亚胺硅氧烷固相微萃取涂层的制备及其在药品残留溶剂分析中的应用分析

Preparation of Polyimide Siloxane Solid Phase Microextraction Coating and its Application Analysis of Residues Solvent in Drugs

目的:探讨制备聚酰亚胺硅氧烷固相微萃取涂层方法和在药品残留溶剂测定中的应用情况。方法:采用分析纯硝基苯、二甲基亚砜、间二甲苯对固相微萃取头,获取聚酰亚胺硅氧烷固相微萃取涂层,并用于药品残留溶剂的分析。结果:取6份溶剂残留量已知样品,将浓度为3.44μg/ml的二甲苯、浓度为4.40μg/ml的二甲基亚砜、浓度为4.80μg/ml的硝基苯各取5ml加入,开展顶空进样分析操作,其中间二甲苯回收率为98.8%,硝基苯回收率为100%,二甲基亚砜回收率为98.9%。精密度分别为2.1%,2.9%,3.6%。结论:表明聚酰亚胺硅氧烷固相微萃取涂层的制备实验方法,具较高准确性和灵敏度,在药品硝基苯、二甲基亚砜、二甲苯残留量的测定中较为适用,可为临床提供有力参考依据。

Objective： To investigate the preparation method of polyimide siloxane solid phase microextraction coating and its ap- plication in the determination of residual solvents in Drugs. Methods： By using and analysing pure nitrobenzene, Dimethyl sulfoxide and m-xylene for solid phase microextraction ,and obtained polyimide siloxane solid phase microextraction coating and used for analy- sis of residues solvent in drugs. Results： Taking 6 known samples of residual solvents ,then added 5ml each of the concentration of 3.44 μg/ml of dimethylbenzene, the concentration of 4.40 μg/ml of dimethyl sulfoxide, the concentration of 4.80 μg/ml nitroben- zene , then Headspace sampling analysis was carried out, the m-xylenerecovery rate was 98.8% and the nitrobenzene recovery rate was 100%. Dimethyl sulfoxide recovery rate was 98.9%. The precision was 2.1%, 2.9%, 3.6% respectively. Conclusions： The result suggests that the experiment method of preparing polyimide siloxane solid phase microextraction coating has high accuracy and sensi- tivity and it is suitable for determining nitrobenzene,Dimethyl sulfoxide, xylene residual quantity in drugs, It can provide useful refer- ence for the clinical.