一种新的保健食品安全监测手段质量轮廓技术

A new method for safety monitoring of natural dietary supplements —quality profile

目的提出有效监控保健食品安全的新方法质量轮廓技术，力图将违禁药物的监控由被动转为主动，有效保障保健食品的安全。方法以高效液相色谱和直接电喷雾质谱法初步研究质量轮廓技术。高效液相色谱法采用0．05％磷酸水和乙腈作为流动相，在c，。柱上全梯度洗脱，以223nm为检测波长，对减肥和降糖保健食品进行化学成分轮廓分析，考察6份不同批号减肥样品A和降糖样品B的高效液相色谱质量轮廓稳定性。在保健食品中分别添加酚酞、西布曲明、罗格列酮、格列本脲、格列齐特，分析质量轮廓中出现的异常成分；另外直接电喷雾质谱法采用ESI＋采集模式，毛细管电压：3．5kV，锥孔电压：30V，萃取电压：4V，聚焦电压：0．5V，源温度：105℃，脱溶剂温度：300oC，脱溶剂气流速：260L/h，锥孔气流速：50L/h，扫描范围：m／z 100—600。考察减肥保健食品C中添加单去甲基西布曲明时，质量轮廓中的异常成分。结果高效液相色谱质量轮廓具有一定的稳定性（色谱相似度大于0.877），且高效液相色谱质量轮廓对保健食品中混入的酚酞、西布曲明、罗格列酮、格列本脲、格列齐特均有反应，直接电喷雾质谱质量轮廓也能明确反映保健食品中混入的单去甲基西布曲明。结论质量轮廓技术可有效监控保健食品中违禁药物的添加情况，防止有害成分的“证后”添加。

Objective A new method for safety monitoring of natural dietary supplementsquality profile was proposed. It would convert passive monitoring of synthetic drug to active, and guarantee the security of natural dietary supplements, Preliminary research on quality profile was completed by high performance liquid chromatography （HPLC） and mass spectrometry （MS）. Methods HPLC was employed to analyze chemical constituent profiles of natural dietary supplements. The separation was completed on Cls column with acetonitrile and water （0.05% HsPO4 ） as mobile phase, the detection wavelength was 223 nm. Based on HPLC, stability of quality profile had been studied, and abnormal compounds in quality profile had been analyzed after addition of phenolphthalein, sibutramine, rosiglitazone, glibenclamide and gliclazide. And by MS, detector worked with ESI ＋, capillary voltage： 3.5 kV, cone voltage： 30 V, extractor voltage ： 4 V, RF lens voltage ： 0. 5 V, source temperature ： 105℃, desolvation temperature ： 300℃, desolvation gas flow rate： 260 L/h, cone gas flow rate： 50 L/h, full scan mass spectra： m/z 100- 600. Abnormal compound in quality profile had been analyzed after addition of N-mono-desmethyl sibutramine. Results Quality profile based on HPLC had good stability （ Similarity 〉 0. 877 ）. Addition of phenolphthalein, sibutramine, rosiglitazone, glibenclamide and gliclazide in natural dietary supplements could be reflected by HPLC, and addition of N-mono-desmethyl sibutramine in natural dietary supplements could be reflected by MS. Conclusion Quality profile might monitor adulteration of natural dietary supplements, and prevent addition of synthetic drug after ＂approval＂.