中空纤维膜液相微萃取-车载HPLC快速筛查七类非法添加药物的方法研究

目的: 在现有药品检测车的基础上,将在固定实验室内静态使用的高效液相色谱仪进行研制改造,加载到现已运行的药品检测车里,和近红外光谱仪联合使用,利用中空纤维膜液相微萃取技术,建立了快速筛查复方化学药品及中成药等各种类型的药品中7类非法添加药物的方法。 方法: 色谱柱:十八烷基硅烷键合硅胶为填充剂,Kromasil C₁₈(250 mm×4.6 mm,5 μm), 以0.01 mol·L^-1乙酸胺-乙腈为流动相,用3种比例(90∶10;50∶50;20∶80)即可对7类物质进行检测,所测成分均具有较好的分离度与较高的理论塔板数。 结果: 检验了包括片剂、胶囊剂、丸剂、颗粒剂和搽剂共48批样品。检出非法添加西药9批,其中壮阳类5批、健胃类2批、镇痛类1批、镇咳平喘1批。 结论: 通过中空纤维膜液相微萃取后,能有效地去除中药及保健食品中的干扰物质,样品处理无需经过中性氧化铝柱纯化,获得了较高的选择性。该方法适合车载环境、快速、简便、准确可靠,可实现在基层现场对假药进行快速试验筛查。

Objective: On the base of present mobile laboratory,HPLC in static state was alterated,equipped on a mobile vehicle,and united with a NIR(near infrared) spectrograph to use.By using hollow fiber based microextraction,the method was established inspecting seven styles of illegal adding in all kinds of medicine such as compound chemicals and Chinese patent drugs. Methods :Chromatographic column Kromasil C₁₈(250 mm×4.6 mm,5 μm),with the mobile phase 0.01 mol·L^-1 ammonium acetate-acetonitrile.The ratio was 90∶10,50∶50,20∶80,and the seven materials would be detected.The detected compoents had good resolutions and remarkable theoretical plate numbers. Results :48 batches were inspected,including tablet,capsule,pill,granules and embrocation.Nine batches of illegal adding in Western medicine were detected,including five batches of aphrodisiac,two batches of stomachicus,a batch of analgetic,a batch of antitussive. Conclusion :By using hollow fiber based microextraction,interference for the determination of Traditional Chinese Medicine and Healthy Food were eliminated effectively.The method is applicable on the mobile vehicle.It is fast,simple and accurate.It can screen and detect false drugs quickly on grass root spots,and enhance effectively supervision,examination frequency and density,in order to ensure the peoples taking medicine security.