解吸附电晕束电离质谱法快速检测中成药及保健食品中非法添加的β-受体阻滞剂

Rapid Determination of Illegally Added β-Receptor Blockers in Traditional Medicines and Dietary Supplements by DCBI-MS Method

建立了新型的解吸附电晕束离子源耦合离子阱质谱法(DCBI-MS),在无需复杂的样品前处理及色谱分离的条件下,可快速检测降血压中成药及保健食品中非法添加的7种β-受体阻滞剂阿替洛尔、比索洛尔、美托洛尔、普萘洛尔、盐酸塞利洛尔、盐酸贝凡洛尔和卡维地洛.采用一级质谱快速筛选和二级质谱确证的方法对目标化合物进行了定性和半定量测定.各目标物的检出限均低于0.1 mg/L,在0.5～100 mg/L浓度范围内线性关系良好.实验获得的7种β-受体阻滞剂的裂解规律为芳氧丙醇胺类化合物的质谱检测提供了参考依据.通过与高效液相色谱-电喷雾离子化质谱法(HPLC-ESI/MS)对比表明,DCBI-MS方法的检测结果可靠.对9种市售样品进行检测,有1批次中成药检出含有未标示的卡维地洛.结果表明,DCBI-MS法测定单个样品的时间不超过1 min,分析速度快,可以在大批量复杂基质样品中β-受体阻滞剂的筛查和药品品质的在线监测中发挥重要作用.

A new rapid method was developed by coupling desorption corona beam ionization to ion trap mass spectrometer（DCBI-MS）.Seven β-receptor blockers,i.e.,atenolol,bisoprolol,metoprolol,propranolol,celiprolol hydrochloride,bevantolol hydrochloride and carvedilol that used be added illegally in antihyperten-sive traditional medicines and dietary supplements were detected.MS1 and MS2 spectra of the sample were employed for rapid screening and semi-quantitation of the target compound.Each aliquot was analyzed in 1 min.The limit of quantification（LOD） of analytes were all less than 0.1 mg/L and the dynamic linear range was 0.5—100 mg/L.The qualitative and semi-quantitative results were confirmed with the traditional HPLC-MS.With the proposed DCBI-MS method,one of 9 real samples was detected to contain the illicit additive of carvedilol.Both in quality control and illicit additive screening of the β-receptor blockers,the DCBI-MS technique can be a powerful tool due to its convenience and specificity.