加校正因子的主成份自身对照法测定达泊西汀中杂质3-氯苯丙醇和甲奈酚

目的建立液相色谱-加校正因子的主成份自身对照法测定达泊西汀中杂质3-氯苯丙醇和甲奈酚的方法。方法色谱柱INTERSIL C 18(2.1 mm×150 mm,3μm);磷酸盐缓冲液(pH=7.5)为流动相A,乙腈为流动相B,进行梯度洗脱;流速为0.8 mL·min-1;检测波长为210 nm。结果3-氯苯丙醇和甲奈酚的校正因子分别为2.8、0.53。达泊西汀、3-氯苯丙醇和甲奈酚的质量浓度在(0.265~0.795)μg·mL-1、(0.260~0.780)μg·mL-1、(0.263~0.788)μg·mL-1范围内与峰面积呈良好的线性关系(r均不低于0.9995),3-氯苯丙醇和甲奈酚检出限分别为0.065μg·mL-1、0.016μg·mL-1,3-氯苯丙醇和甲奈酚平均回收率分别为97.2%(RSD=1.2%)、99.2%(RSD=0.6%)。结论本方法灵敏、准确,可作为达泊西汀中杂质3-氯苯丙醇和甲奈酚含量测定。

New Constituents from the Fresh Stems of Opuntia Dillenii

Aim To study the chemical composition of Opuntia dillenii Haw. Methods Manykinds of chromatogra-phy methods were used in the isolation procedure, while the structures ofisolated compounds were determined on the aids of NMR and MS spectral analysis. Result Three newcompounds, together with 14 known compounds, were isolated form the 80% ethanolic extract of itsstems. Conclusion The three new compounds, opuntioside Ⅰ (2), 4-ethoxyl-6-hydroxymethyl-α-pyrone(3) and kaempferol 7-O-β-D-glucopyranosyl (1→4)-β-D-glucopyranoside (4), were characterized.