中药及保健食品中PDE5抑制剂检测方法研究及未知衍生物的发现

 目的为打击中药制剂及保健食品中非法添加化学药物现象,针对常见的5型磷酸二酯酶(PDE5)抑制剂,研究建立了快速理化鉴别方法和HPLC-MS/MS方法。方法采用Waters Sunfire C₁₈色谱柱,梯度洗脱:流动相A为20 mmol·L^-1醋酸铵溶液,流动相B为甲醇-乙腈(2∶1),检测波长为230 nm,流速为1 mL·min^-1(分流比为4∶1)。选择正负离子全扫描方式检测。结果在上述色谱及质谱条件下,对于常见的3种PDE5抑制剂进行了质谱裂解规律的分析总结,并用于未知衍生物的结构推测,成功检测出3个衍生物,其中一个结构未见报道,本所根据核磁共振图谱确定了结构。结论该方法简便,快捷、灵敏度、准确性、重现性均可满足定性检查的要求。

Study on PDE5 Inhibitors and Its Unknown Derivatives in Traditional Chinese Medicine and Health Food Discovered

OBJECTIVE To develop a high performance liquid chromatography assay with electrospray ion trap mass spectrometry(Finnigan LCQ) identify chemical medicines illegally adulterated in traditional Chinese medicine(TCM) preparations,a method for the analysis of PDE₅ inhibitors in Chinese medicine and health food.METHODS The fragmentation pattern of these drugs was summarized.After being separated by HPLC,the organic solvent extraction from TCM preparations was analyzed by the mass spectrometer,operated in positive ion or negative mode and in three scan modes including full scan MS,selected ion monitoring and full scan MS2.The obtained pseudomolecular ions and fragment ions were used to identify these drugs.RESULTS HPLC MS resolution of above five PDE5 inhibitors were good.CONCLUSION The methed offers advantages was specific,quick and sensitive.