摘要
目的:建立一测多评法同时测定制川乌中9种乌头类生物碱含量。方法:采用高效液相色谱四级杆飞行时间串联质谱(HPLC-QTOF-MS)法。色谱柱为Agilent ZORBAX Extend-C_(18)RRHT(2.1 mm×50 mm,1.8μm);甲醇为流动相A,以水(含0.1%甲酸和2.5 mmol·L^(-1)醋酸铵溶液)为流动相B,梯度洗脱;流速为0.21 mL·min^(-1);柱温为30℃。以乌头碱为内参物,测定次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱、乌头原碱、次乌头原碱、新乌头原碱对于其的相对校正因子,并对相对校正因子进行重现性考察。利用相对校正因子计算其它8种生物碱成分的含量,同时利用外标法测定这9种成分,比较两种测定方法的差异,验证一测多评法的准确性和可行性。结果:建立QAMS法测定乌头类中药材9种生物碱的含量,其测定值与计算值无显著差异。结论:经方法学验证,本方法可用于制川乌药材中9种生物碱的含量测定。
Objective： To develop a method for the quantitative analysis of multi-components by single marker （ QAMS） for nine alkaloids in Radix Aconiti Praeparata. Methods： An HPLC-QTOF-MS method with an Agilent ZORBAX Extend-C18 RRHT column （2.1mm×50 mm, 1.8μm） was applied. The flow rate was 0.21mL-min_1. The column temperature was 30 The mobile phase was methanol （ A）-water （ contain-ing 0.1% formic acid and 2.5 mmol · L-1 ammonium acetate） （ B） in gradient elution. Aconitine was used as internal reference substance, to respectively establish the relative correction factor （ RCF） of hypaconitine, mesaconitine, benzoylaconine, benzoylhypaconine, benzoylmesaconine, aconine, hypaconine and mesaconine, and inspect the reproducibility of RCFs; the contents of the other 8 aconitum alkaloids were calculated ac-cording to the RCFs, respectively. At the same time, an external standard method （ ESM） was performed for the content determination of the nine alkaloids. The two methods were compared. The feasibility and accu-racy of the QAMS method were verified. Results： The QAMS method was established for determining alka-loids. There was no significant difference between the QAMS method and the external standard method （ ESM）. Conclusion： With the validation of methodology, the method established in our study can be used for content determination of aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylhypaconine, ben- zoylmesaconine, aconine, hypaconine and mesaconine.
出处
《药学与临床研究》
2017年第2期113-116,162,共5页
Pharmaceutical and Clinical Research
基金
江苏省中医药局科技项目(YB2015121)
关键词
制川乌
一测多评法
乌头类生物碱
相对校正因子
外标法
含量测定
Radix Aconiti Praeparata
Quantitative analysis of multi -components by single marker （ QAMS）
Aconitum alkaloid
Relative correction factors
External standard method
Quanititative determination162
