Wang Wei, Li Chang-Yin, Wen Xiao-Dong, Li Ping, Qi Lian-Wen
Key Laboratory of Modern Chinese Medicines (China Pharmaceutical University), Ministry of Education; Nanjing, 210009, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Mar 15;877(8-9):671-9. doi: 10.1016/j.jchromb.2009.01.021. Epub 2009 Jan 23.
A rapid high-performance liquid chromatography-mass spectrometry (HPLC-MS) method was developed and validated for simultaneous quantification of 6-gingerol, 8-gingerol, 10-gingerol and 6-shogaol in rat plasma after oral administration of ginger oleoresin. Plasma samples extracted with a liquid-liquid extraction procedure were separated on an Agilent Zorbax StableBond-C(18) column (4.6 mm x 50 mm, 1.8 microm) and detected by MS with electrospray ionization interface in positive selective ion monitoring (SIM) mode. Calibration curves (1/x(2) weighted) offered satisfactory linearity (r(2)>0.995) in a wide linear range (0.0104-13.0 microg/mL for 6-gingerol, 0.00357-4.46 microg/mL for 8-gingerol, 0.00920-11.5 microg/mL for 10-gingerol and 0.00738-9.22 microg/mL for 6-shogaol). The lower limit of quantification (LLOQ) was in a range of 3.57-10.4 ng/mL. The analytes and internal standard can be baseline separated within 6 min. Inter- and intra-day assay variation was less than 15%. This developed method was successfully applied to pharmacokinetic studies of ginger oleoresin after oral administration to rats. Glucuronide of 6-gingerol was determined after beta-glucuronidase hydrolysis for more information, and the intestinal glucuronidation was further confirmed by comparison of plasma samples of hepatic portal vein and femoral vein.
建立了一种快速高效液相色谱-质谱联用（HPLC-MS）方法，并对其进行了验证，用于同时定量大鼠口服姜辣素后血浆中的6-姜酚、8-姜酚、10-姜酚和6-姜烯酚。采用液-液萃取法提取的血浆样品在Agilent Zorbax StableBond-C(18)柱（4.6 mm×50 mm，1.8 µm）上进行分离，并通过质谱在正离子选择离子监测（SIM）模式下的电喷雾电离接口进行检测。校准曲线（1/x(2)加权）在较宽的线性范围内（6-姜酚为0.0104-13.0 μg/mL，8-姜酚为0.00357-4.46 μg/mL，10-姜酚为0.00920-11.5 μg/mL，6-姜烯酚为0.00738-9.22 μg/mL）提供了令人满意的线性（r(2)>0.995）。定量下限（LLOQ）在3.57-10.4 ng/mL范围内。分析物和内标可在6分钟内实现基线分离。日内和日间测定变异小于15%。该方法成功应用于大鼠口服姜辣素后的药代动力学研究。为获取更多信息，在β-葡萄糖醛酸酶水解后测定了6-姜酚的葡萄糖醛酸苷，并通过比较肝门静脉和股静脉的血浆样品进一步证实了肠道葡萄糖醛酸化。
