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目的:建立同时测定白香丹胶囊中芍药苷、丹皮酚和α-香附酮在人血浆中含量的方法并测定其体外血浆蛋白结合率。方法:采用平衡透析法计算血浆蛋白结合率。样品经乙酸乙酯萃取,采用LC-MS/MS检测,Phenomenex Luna C18色谱柱(2.0 mm×100 mm,3μm),流动相甲醇-0.1%甲酸水(含2 mmol·L~(-1)甲酸铵)(80∶20),流速0.2 m L·min~(-1)。离子化模式为正离子,定量模式多反应监测模式,毛细管电压4 kV,干燥气温度400℃。检测对象芍药苷m/z 503.2~503.2,裂解电压200 V,碰撞电压0 V;丹皮酚m/z 167.1~120.9,裂解电压100 V,碰撞电压20 V;α-香附酮m/z 218.9~111.0,裂解电压100 V,碰撞电压20 V;毛蕊异黄酮(内标)m/z 285.1~213.1,裂解电压170 V,碰撞电压40 V。结果:白香丹胶囊在低、中、高(56.2,112.5,168.8 mg·L~(-1))质量浓度下,芍药苷的血浆蛋白结合率分别为(24.82±3.91)%,(20.88±2.69)%,(22.40±3.33)%,丹皮酚分别为(88.62±1.68)%,(86.16±2.36)%,(88.73±0.80)%,α-香附酮依次为(80.69±1.12)%,(78.10±2.28)%,(72.57±0.30)%。结论:白香丹胶囊中主要成分芍药苷、丹皮酚及α-香附酮与人血浆蛋白结合率大小排序为丹皮酚>α-香附酮>芍药苷。
OBJECTIVE: To establish a method for the simultaneous determination of paeoniflorin, paeonol and alpha-ketodone in human plasma in Bai Xiang Dan Capsule and to determine the in vitro plasma protein binding rate. Methods: Balanced dialysis was used to calculate the plasma protein binding rate. The sample was extracted with ethyl acetate and detected on a Phenomenex Luna C18 column (2.0 mm × 100 mm, 3 μm) using mobile phase of methanol-0.1% formic acid (containing 2 mmol·L -1 formic acid) Ammonium (80:20) at a flow rate of 0.2 m L · min ~ (-1). Ionization mode is positive ion, quantitative mode multi-reaction monitoring mode, capillary voltage 4 kV, drying gas temperature 400 ℃. Paeoniflorin (m / z 503.2 ~ 503.2), cleavage voltage 200 V, collision voltage 0 V, paeonol m / z 167.1 ~ 120.9, lysis voltage 100 V and collision voltage 20 V; ~ 111.0, lysis voltage 100 V, collision voltage 20 V; calycosin (internal standard) m / z 285.1 ~ 213.1, lysis voltage 170 V and collision voltage 40 V. Results: The plasma protein binding rates of paeoniflorin were (24.82 ± 3.91)% and (20.88 ±)%, respectively, at low, medium and high concentrations (88.62 ± 1.68)%, (86.16 ± 2.36)% and (88.73 ± 0.80)%, respectively, and the values of α-ketones were (80.69 ± 1.12)% and (22.40 ± 3.33)%, , (78.10 ± 2.28)%, (72.57 ± 0.30)% respectively. Conclusion: The main components of paeoniflorin paeoniflorin, paeonol and α-ketones and human plasma protein binding rate of the order of paeonol> α-ketones ketone> paeoniflorin.