搭建了电喷雾离化离子迁移率谱(ESI-IMS)与高效液相色谱(HPLC)的联用系统并对降糖类保健品添加物进行检测。制备了可调针阀型分流器调节和控制ESI-IMS进样流速;选用金属毛细管电喷针,增大产生稳定电喷雾的流速范围;使用水冷装置,改善电喷雾稳定性和去溶剂化效果;采用90%甲醇溶液作为流动相对5种降糖药标准品混合溶液进行检测,缩短HPLC保留时间,检测限达到50μg/L。应用联用系统对中成药消渴丸和5种降糖类保健品进行分析,检测时间小于8 min;在2种保健品中发现了添加的苯乙双胍和二甲双胍药物成分,实现了降糖类保健品中非法添加物的快速测定。
A combined system of electrospray ionization- ion mobility spectrometer( ESI-IMS) and high performance liquid chromatograph( HPLC) was built up to detect anti-diabetic health care products. An adjustable splitter with a needle inserted in a tee-piece after the column was prepared for the change of flow rate. The stainless steel capillary was used as electrospray needle to broaden the range of flow rate. Stable electrospray ionization and good desolvation effect were obtained by using a water cooling device. The mixture of five anti-diabetic standards was analyzed with the mobile phase of 90% methanol solution by the HPLC-ESIIMS system,which shortened the detected time. The limit of detection for metformin can reach 50 μg / L. One anti-diabetic herbal medicine and five health care products were analyzed by the HPLC-ESI-IMS,the detection time of each substance was 8 min; Metformin and Phenformin were measured in two of the five health care products. The experimental results demonstrate that rapid determination of illegal additives in health care products can be realized by the HPLC-ESI-IMS system.