UPLC-MS/MS法测定槲寄生抗肿瘤成分1,7-bis(4-hydroxyphenyl)-1,4-heptadien-3-one的含量  

Determination of cytotoxic constituent 1,7-bis(4-hydroxyphenyl )-1,4-heptadien-3-one of Viscum coloratum by UPLC-MS/MS

作　　者：张照燕[1] 龙猜 田秀敏 于治国[1] 党晓伟[2] 赵云丽[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]承德护理职业学院,河北承德067000

出　　处：《沈阳药科大学学报》2018年第1期53-57,共5页Journal of Shenyang Pharmaceutical University

基　　金：沈阳市重点科技研发计划资助项目(17-126-9-00)

摘　　要：目的建立超高效液相色谱-串联质谱法(UPLC/MS/MS)测定槲寄生中具有抗肿瘤活性的新化合物1,7-bis(4-hydroxyphenyl)-1,4-heptadien-3-one(BHPHD)的含量,并通过多因素方差分析比较产地与寄主对药材抗肿瘤成分含量的影响。方法以Thermo Hypersil GOLD C18(50 mm×2.1 mm,1.9μm)为分离色谱柱,乙腈-体积分数0.1%甲酸水溶液为流动相,流速0.2 m L·min-1,梯度洗脱,质谱检测器,电喷雾正离子,多反应监测模式,监测离子对m/z 295.09→106.99。结果BHPHD在质量浓度为0.050~2.5 mg·L-1内线性关系良好,精密度、重复性、稳定性试验的RSD均≤3.5%,平均加样回收率(n=9)为97.2%(RSD=1.6%)。结论该方法可满足定量要求。多因素方差分析表明槲寄生中BHPHD的含量受产地影响较大(P<0.01),受寄主影响不大。Objective To establish a method for determination of the cytotoxic constituent 1,7-bis （4- hydroxyphenyl）-l, 4-heptadien-3-one （BHPHD）of Viscum coloratura by ultra performance liquid chromatography-tandem mass spectrometric （UPLC-MS/MS）. And to evaluate the influence of source and host on the content of the cytotoxic constituent by multiple factors analysis of variance. Methods Chromatographic analysis was carded out on a Thermo Hypersil GOLD C18 colulnn （50 mm× 2. 1 mm, 1.9 μm）. The mobile phase was composed of acetonitrile and 0. 1% （V： V）formic acid in water. Gradient elution was applied, and the flow rate was 0. 2 mL. min- 1. BHPHD was detected by positive electrospray ionization in multiple reaction monitoring mode, and the ion transition monitored was m/z 295.09---106. 99. Results The linear range of calibration curve was 0. 050 - 2.5 mg · L-1. The RSDs of precision, reproducibility and stability tests were all no more than 3.5%, and the average recovery was 97.2% with RSD of 1.6% （n =9）. Conclusions The method is sensitive, accurate, and fast, which can be used to determine the content of BHPHD in Viscum coloratura. The results of multiple factors analysis of variance indicated that the source of Viscum coloratum had a significant impact on the BHPHD content（ P 〈0. 01 ）. In contrast, the host species were not the main factor.

关 键 词：槲寄生 1 7-bis(4-hydroxyphenyl)-1 4-heptadien-3-one 超高效液相色谱-串联质谱 含量测定 

分 类 号：R917[医药卫生—药物分析学]