目的:建立一个灵敏、快速、可靠的HPLC-Ms法,以对乙酰氨基酚为内标(IS),同时测定白术内酯I、Ⅱ、Ⅲ(AT-I、Ⅱ、Ⅲ)及其在大鼠体内的药动力学研究。方法:血浆样品经乙酸乙酯萃取后,使用HPLC-MS法,ZORBAXSB-C18色谱柱(3.5um,2.1×100mm),柱温35℃,流动相为甲醇:0.1%甲酸水(85:15),流速为0.4ml/min;采用正离子模式MRM检测。结果:白术内酯I、Ⅱ、Ⅲ的方法学验证(专属性、线性、检测灵敏度、准确度与精密度、基质效应与提取回收率、稳定性)良好,并成功应用于给药白术药材及白术.麻黄(4:3)药材提取物后大鼠体内的药代动力学研究。结论:本方法可用于白术及其体内的药动学研究,为临床合理使用白术药材提供一定的参考价值。
Objective: A sensitive, rapid and reliable HPLC-MS method was developed for doing the simultaneous determination of atractylenolide I , atractylenolide II and atractylenolide III ( AT- I , II, III ) in rat plasma and its application to pharmaeokinetic study using paracetamol as internal standard(IS). Methods:Rat plasma samples were extracted with ethyl acetate. The analytes were separated on a Zorbax SB-C18 column (2.1 × 100mm,3. Sum), column temperature for 35℃, eluting with Solvent A( 85% Me)and Solvent B (15 % 0.1% formic-water) at the flow rate of 0.4 ml/min, the detection performed by positive ion, multiple reaction monitoring (MRM) mode. Results:The methodology validation of atractylenolide I , atractylenolide II and atractylenolide III was good ( specificity, linear, detection sensitivity, accuracy and precision,matrix effect and extract recovery, stability), and the validated method was successfully applied to the pharmacokinetic study after the rice oral administration of Atractylodes macrocephala Rhizoma (AMR) extract and Atractylodes macrocephala Rhizoma-Herba Ephedrae (4: 3) extract. Conclusion:This method was available for pharmacokinetic study after oral administration of AMR , and possibly provided a meaningful basis for clinical fair use of AMR.