中国药房2018，Vol.29Issue(6)：761-765,5.DOI:10.6039/j.issn.1001-0408.2018.06.10
高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法快速检测大鼠血浆中6种附子生物碱
Rapid Determination of 6 Kinds of Aconite Alkaloids in Rat Plasma by HPLC-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
摘要
Abstract
OBJECTIVE:To establish HPLC-quadrupole/electrostatic field orbitrap high resolution mass spectrometry for rapid determination of aconitine,mesaconitine,hypaconitine,benzoylaconitine,benzoylmesaconine and benzoylhypacoitine in rat plasma. METHODS:Internal standard lappaconitine was added into plasma sample,and methanol precipitated protein was used for pretreatment. HPLC-quadrupole/electrostatic field orbitrap high resolution mass spectrometry was adopted. HPLC condition was as follows as Sinochrom ODS-BP C18column,mobile phase consisted of acetonitrile-1% formic acid solution(50:50,V/V),the flow rate of 0.6 mL/min,sample size of 10 μL,column temperature of 25 ℃,automatic sampler temperature of 4 ℃. Mass spectrum scanning mode was full ion monitoring model,positive ion acquisition,mass charge ratios(m/z)of ion were 646.32(aconitine), 632.30(mesaconitine),616.31(hypaconitine),604.31(benzoylaconitine),590.29(benzoylmesaconine),574.30(benzoylhypacoitine), 585.31(internal standard). Six male Wistar rats were collected and given single dose of total alkaloid extract of Aconitum carmichaeli(4 mg/kg)intragastrically. Blood samples were collected before medication(0 h)and 0.5,0.75,1.25,1.5,2,4,6, 8,10,24 h after medication. Plasma concentration was determined and pharmacokinetic parameters were calculated by using PK-Solver V2.0 software. RESULTS:The linear range of 6 kinds of aconitum alkaloids in plasma were 0.1-10 μ g/L(r>0.992). The limit of quantitation was 0.1 μ g/L. Average recovery was higher than 75%,RSDs of intra-day and inter-day,matrix effects,stability test were all lower than 15%. The tmaxof 6 kinds of aconite alkaloids were about 1.2 h;t1/2were about 10 h;cmaxof monoestertype aconite alkaloids were higher than those of diester-type aconite alkaloids. CONCLUSIONS:Established HPLC-quadrupole/electrostatic field orbitrap high resolution mass spectrometry is accurate,sensitive,simple and rapid, and can be used for plasma concentration monitoring of 6 kinds of aconitum alkaloids.关键词
高效液相色谱法/四极杆/静电场轨道阱高分辨率质谱法/附子生物碱/血药浓度/大鼠Key words
HPLC/Quadrurpole/electrostatic field orbitrap mass spectrometry/Aconitum alkaloids/Plasma concentration/Rats分类
医药卫生引用本文复制引用
赛那,金蓉,布仁,顾艳丽,林英华,雷雯朴,孙耀..高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法快速检测大鼠血浆中6种附子生物碱[J].中国药房,2018,29(6):761-765,5.基金项目
内蒙古自治区蒙医药协同创新培育中心研究项目(No.MYYXT201705) （No.MYYXT201705）
内蒙古医科大学实验室开放基金项目(No.2016ZN16) （No.2016ZN16）
