沈阳药科大学学报

2018, v.35;No.264(01) 53-57

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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

张照燕,龙猜,田秀敏,于治国,党晓伟,赵云丽
ZHANG Zhaoyan,LONG Cai,TIAN Xiumin,YU Zhiguo,DANG Xiaowei,ZHAO Yunli

摘要(Abstract):

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)-1,4-heptadien-3-one( BHPHD) of Viscum coloratum 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 w as carried out on a Thermo Hypersil GOLD C18 column( 50 mm × 2. 1 mm,1. 9 μm). The mobile phase w as composed of acetonitrile and 0. 1%( V ∶ V) formic acid in w ater. Gradient elution w as applied,and the flow rate w as 0. 2 m L·min-1. BHPHD w as detected by positive electrospray ionization in multiple reaction monitoring mode,and the ion transition monitored w as m/z 295. 09→106. 99.Results The linear range of calibration curve w as 0. 050-2. 5 mg · L-1. The RSDs of precision,reproducibility and stability tests w ere all no more than 3. 5%,and the average recovery w as 97. 2% w ith RSD of 1. 6%( n = 9). Conclusions The method is sensitive,accurate,and fast,w hich can be used to determine the content of BHPHD in Viscum coloratum. 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 w ere not the main factor.

关键词(KeyWords): 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
Viscum coloratum;1,7-bis(4-hydroxyphenyl)-1,4-heptadien-3-one;ultra performance liquid chromatography-tandem mass spectrometry(UPLC/MS/MS);content determination

Abstract:

Keywords:

基金项目(Foundation): 沈阳市重点科技研发计划资助项目(17-126-9-00)

作者(Author): 张照燕,龙猜,田秀敏,于治国,党晓伟,赵云丽
ZHANG Zhaoyan,LONG Cai,TIAN Xiumin,YU Zhiguo,DANG Xiaowei,ZHAO Yunli

DOI: 10.14066/j.cnki.cn21-1349/r.2018.01.010

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