超高效液相色谱串联质谱法测定木香马兜铃中马兜铃酸Ⅰ及马兜铃酸Ⅱ的含量

目的:建立测定木香马兜铃中马兜铃酸Ⅰ(AA-Ⅰ)及AA-Ⅱ含量的超高效液相色谱-质谱法。方法:色谱柱为Agilent Poroshell SB-C18(100 mm×2.1 mm,2.7μm),流动相为乙腈-0.1%甲酸水溶液(含5 mmol·L^(–1)甲酸铵),梯度洗脱,流速0.3 mL·min^(–1),柱温35℃,离子源为电喷雾离子源,扫描方式为正离子扫描,多反应离子监测模式。结果:AA-Ⅰ在质量浓度为1.036~207.310 ng·mL^(–1)时与峰面积线性关系良好(r=0.9995);AA-Ⅱ在质量浓度为1.1~110.0 ng·mL^(–1)时与峰面积线性关系良好(r=0.9991);AA-Ⅰ的定量限、检测限分别为0.3287、0.0986 pg;AA-Ⅱ的定量限、检测限分别为0.6506、0.1952 pg;AA-Ⅰ的精密度、稳定性、重复性试验RSD均小于5.0%;AA-Ⅱ的精密度、稳定性、重复性试验RSD均小于5.0%;AA-Ⅰ的平均加样回收率为92.50%,RSD为4.3%;AA-Ⅱ的平均加样回收率为104.97%,RSD为3.7%。15批木香马兜铃药材中1批未检出AA-Ⅰ,8批未检出AA-Ⅱ,其余批次的AA-Ⅰ质量分数为5.94×10^(–4)~2.86 mg·g^(–1),AA-Ⅱ质量分数为0.09~0.50 mg·g^(–1)。结论:所建立的方法专属性强、快速、灵敏,可用于木香马兜铃中AA-Ⅰ及AA-Ⅱ的含量测定。

木香马兜铃与七味红花殊胜丸中马兜铃酸A测定研究

目的建立HPLC法测定木香马兜铃及七味红花殊胜丸中马兜铃酸A。方法采用HPLC法,Sunfire-ODS C18(5μm,250 mm×4.6 mm)色谱柱;流动相为乙腈-0.05%磷酸溶液(45∶55);检测波长为322 nm。结果马兜铃酸A在0.014 8～0.294μg(r=0.999 9)的范围内线性关系良好;平均回收率为98.9%,RSD为1.0%。结论本法操作简便,准确性、重复性好,可用于木香马兜铃与七味红花殊胜丸中马兜铃酸A的测定。

HPLC测定二十五味余甘子丸中的马兜铃酸Ⅰ

目的采用HPLC法检测二十五味余甘子丸中马兜铃酸Ⅰ的限量。方法采用Waters Sunfire C18色谱柱(250 mm×0.46 mm,5μm),检测波长为250 nm,流动相为0.05%磷酸溶液-乙腈(60∶40),进样量10μL。结果0.195~4.87μg·mL^-1马兜铃酸Ⅰ与峰面积的线性关系良好(r2=0.9999),平均回收率为97.17%,RSD=1.45%(n=6);4批样品中马兜铃酸Ⅰ的含量为0~2.85μg·g^-1。结论所用方法简便、快速、重复性好、回收率高、结果可靠,可用于二十五味余甘子丸中马兜铃酸Ⅰ的限量检查。

Pharmacokinetica studies of aristolochic acid-I and-II in rats after intragastrical administration of Radix Aristolochiae and Muskone

The pharmacokinetic parameters of aristolochic acid-Ⅰ （AA-Ⅰ） and -Ⅱ （AA-Ⅱ） in rat serum after intragastrical administration of the crude drug powders of Radix Aristolochiae （RA） and Muskone containing equal amounts of RA were compared. The pharmacokinetic profiles of AA-Ⅰ and AA-Ⅱ could be fitted with a two-compartment model The elimination half time （T1/2β） of AA-Ⅰ in Muskone was 1573.2 min and that of AA-Ⅰ in RA was 475.8 min; T1/2β of AA-Ⅱ in Muskone was 2344.8 min and that of AA-Ⅱ in RA was 427.8 rain. The area under the concentration-time curve （AUC） of AA-Ⅰ in Muskone was 13.07 μg/h/mL and that of AA-Ⅰ in RA was 3.86 μg/h/mL; AUC of AA-Ⅱ in Muskone was 67.67 μg/h/mL and that of AA-Ⅱ in RA was 23.93 μg/h/mL. The bioavailabilities of AA-Ⅰ and AA-Ⅱ in Muskone were markedly increased compared with that in RA based on the elimination half-time and A UC values.