Li Yun-Qing, Li Cheng-Jian, Lv Lei, Cao Qing-Qing, Qian Xian, Li Si Wei, Wang Hui, Zhao Liang
Department of Pharmacy, Shanghai Eastern Hepatobiliary Surgery Hospital, Shanghai, China.
Department of Pharmacy, The Children Hospital of Shanxi, Taiyuan, China.
Biomed Chromatogr. 2018 Jun;32(6):e4189. doi: 10.1002/bmc.4189. Epub 2018 Feb 12.
Stellera chamaejasme L. has been used as a traditional Chinese medicine for the treatment of scabies, tinea, stubborn skin ulcers, chronic tracheitis, cancer and tuberculosis. A sensitive and selective ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the simultaneous determination of five flavonoids (stelleranol, chamaechromone, neochamaejasmin A, chamaejasmine and isochamaejasmin) of S. chamaejasme L. in rat plasma. Chromatographic separation was accomplished on an Agilent Poroshell 120 EC-C column (2.1 × 100 mm, 2.7 μm) with gradient elution at a flow rate of 0.4 mL/min and the total analysis time was 7 min. The analytes were detected using multiple reaction monitoring in positive ionization mode. The samples were prepared by liquid-liquid extraction with ethyl acetate. The UPLC-MS/MS method was validated for specificity, linearity, sensitivity, accuracy and precision, recovery, matrix effect and stability. The validated method exhibited good linearity (r ≥ 0.9956), and the lower limits of quantification ranged from 0.51 to 0.64 ng/mL for five flavonoids. The intra- and inter-day precision were both <10.2%, and the accuracy ranged from -11.79 to 9.21%. This method was successfully applied to a pharmacokinetic study of five flavonoids in rats after oral administration of ethyl acetate extract of S. chamaejasme L.
瑞香狼毒已被用作治疗疥疮、癣、顽固性皮肤溃疡、慢性气管炎、癌症和肺结核的传统中药。建立并验证了一种灵敏且选择性的超高效液相色谱-串联质谱（UPLC-MS/MS）方法，用于同时测定大鼠血浆中瑞香狼毒的五种黄酮类化合物（狼毒素、狼毒色原酮、新狼毒素A、狼毒素和异狼毒素）。色谱分离在安捷伦Poroshell 120 EC-C柱（2.1×100 mm，2.7μm）上进行，采用梯度洗脱，流速为0.4 mL/min，总分析时间为7分钟。采用正离子模式下的多反应监测检测分析物。样品通过乙酸乙酯液-液萃取制备。该UPLC-MS/MS方法在特异性、线性、灵敏度、准确度和精密度、回收率、基质效应和稳定性方面进行了验证。验证后的方法显示出良好的线性（r≥0.9956），五种黄酮类化合物的定量下限范围为0.51至0.64 ng/mL。日内和日间精密度均<10.2%，准确度范围为-11.79至9.21%。该方法成功应用于大鼠口服瑞香狼毒乙酸乙酯提取物后五种黄酮类化合物的药代动力学研究。
