Han De-En, Shi Yanmei, Tian Ping, Wei Hengchao, Miao Mingsan, Li Xiu-Min
College of Pharmacy, Henan University of Chinese Medicine, Zhengzhou, China.
International TCM Immunopharmacology Research Center, Henan University of Chinese Medicine, Zhengzhou, China.
Biomed Chromatogr. 2020 Jul;34(7):e4838. doi: 10.1002/bmc.4838. Epub 2020 May 19.
A rapid and sensitive method was developed and validated for the quantitative determination of xanthopurpurin (XPP) in rat plasma using ultra-performance liquid chromatography-electrospray ionization-Orbitrap mass spectrometry. XPP inhibits IgE production and prevents peanut-induced anaphylaxis. The XPP and emodin (internal standard) were determined in negative ion mode with m/z 239.0350 → 211.0400 and 269.0455 → 241.0507, respectively. The separation process was achieved using an ACQUITY UPLC HSS T column with acetonitrile and 0.1% formic acid in water (85:15). The linear range was 0.5-100 ng/mL, and the correlation coefficient (r ) was > 0.993. The inter-day and intra-day precision was within an acceptable range of 15%. The extraction recovery and matrix effect were 78.9-87.2% and 94.3-98.5%, respectively. Under different conditions, the XPP was stable in the range of 5.6-10.6%. This method was successfully applied to study the pharmacokinetics of XPP with an oral dose of 10.0 mg/kg and intravenous dose of 2.0 mg/kg in rats. The absolute oral bioavailability of XPP was 4.6%.
建立了一种快速灵敏的超高效液相色谱-电喷雾电离-轨道阱质谱法测定大鼠血浆中黄嘌呤紫红素（XPP）的含量，并进行了方法验证。XPP可抑制IgE产生并预防花生诱导的过敏反应。采用负离子模式测定XPP和大黄素（内标），其质荷比分别为m/z 239.0350→211.0400和269.0455→241.0507。使用ACQUITY UPLC HSS T柱，以乙腈和0.1%甲酸水溶液（85:15）进行分离。线性范围为0.5-100 ng/mL，相关系数（r）>0.993。日间和日内精密度在可接受的15%范围内。提取回收率和基质效应分别为78.9-87.2%和94.3-98.5%。在不同条件下，XPP的稳定性在5.6-10.6%范围内。该方法成功应用于研究大鼠口服剂量10.0 mg/kg和静脉注射剂量2.0 mg/kg的XPP的药代动力学。XPP的绝对口服生物利用度为4.6%。
