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目的:建立测定大鼠血浆中白藜芦醇衍生物(E)-3,5,4′-三甲氧基-1,2-二苯乙烯的液相色谱-质谱法(HPLC-MS)定量分析方法。方法:血浆样品0.1 mL,经乙腈沉淀蛋白后,以 ODS Hypersil C_(18)(5 μm,250 mm×4.6 mm)为固定相,甲醇-10 mmol·L~(-1)醋酸铵(0.2%甲酸)(80:20,v/v)为流动相,流速为0.85 mL·min~(-1);采用 HPLC-MS,选择离子监测(SIM)法检测(E)-3,5,4′-三甲氧基-1,2-二苯乙烯([M+H]~+,m/z 271.3),卡马西甲([内标,M+H]~+,m/z 237.5),保留时间分别为8.9,4.0 min。结果:(E)-3,5,4′-三甲氧基-1,2-二苯乙烯的线性范围为0.01～5.0 μg·mL~(-1),r>0.999;日内、日间精密度 RSD 小于12.9%;相对回收率在94.8%～104.7%之间,最低检出限为0.005 μg·mL~(-1)结论:经方法学确证和稳定性评价,该方法成功用于大鼠血浆中(E)-3,5,4′-三甲氧基-1,2-二苯乙烯的定量测定。
Objective: To establish a liquid chromatography-mass spectrometry (HPLC-MS) quantitative analysis of (E)-3,5,4’-trimethoxy-stilbene in resveratrol in rat plasma. method. Methods: Plasma sample 0.1 mL, protein precipitated with acetonitrile, ODS Hypersil C 18 (5 μm, 250 mm×4.6 mm) as stationary phase, methanol-10 mmol·L -1 ammonium acetate (0.2%) Formic acid) (80:20, v/v) is the mobile phase with a flow rate of 0.85 mL·min~(-1). The selected ion monitoring (SIM) method was used for the detection of (E)-3,5,4′ by HPLC-MS. -Trimethoxy-stilbene ([M+H]~+, m/z 271.3), Carmazig ([Internal standard, M+H]~+, m/z 237.5), Retention time They were 8.9, 4.0 min. Results: The linear range of (E)-3,5,4′-trimethoxy-stilbene was 0.01-5.0 μg·mL-1, r>0.999; intra-day and inter-day precision RSD was less than 12.9%; the relative recoveries were between 94.8% and 104.7%, and the limit of detection was 0.005 μg·mL -1. Conclusion: The method was successfully applied to rat plasma after methodological validation and stability evaluation. Quantitative determination of (E)-3,5,4’-trimethoxystilbene.