HPLC-DAD法同时测定苦参配方颗粒中6种生物碱成分的含量  

Simultaneous determination of 6 alkaloid constitutents in Kushen dispensing granule by HPLC-DAD

作　　者：李华丽 王小龙 叶晓娅 LI Hua-li;WANG Xiao-long;YE Xiao-ya(Pingdingshan Food and Drug Inspection Institute, Pingdingshan Henan 46700)

机构地区：[1]平顶山市食品药品检验所中药室,河南平顶山467000

出　　处：《中南药学》2018年第5期687-691,共5页Central South Pharmacy

摘　　要：目的建立HPLC-DAD法同时测定苦参配方颗粒中氧化槐醇碱、氧化苦参碱、槐定碱、氧化槐果碱、苦参碱及槐果碱6种生物碱活性成分的含量。方法 Waters CSH C18色谱柱(4.6 mm×250 mm,5μm),流动相为20 mmol·L^(-1)醋酸铵水溶液(0.1%氨水,p H=9.0)(A)-20 mmol·L^(-1)醋酸铵的甲醇-乙腈(1∶1)混合溶液(B),梯度洗脱,流速0.8 m L·min-1,检测波长220 nm,柱温35℃。结果氧化槐醇碱、氧化苦参碱、槐定碱、氧化槐果碱、苦参碱及槐果碱的质量浓度分别在0.081~1.620μg(r=0.9999)、0.240~4.800μg(r=0.9998)、0.065~1.300μg(r=0.9997)、0.131~2.620μg(r=0.9996)、0.048~0.950μg(r=0.9997)及0.045~0.900μg(r=0.9998)内与峰面积呈良好的线性关系。氧化槐醇碱、氧化苦参碱、槐定碱、氧化槐果碱、苦参碱及槐果碱的平均加样回收率分别为98.2%、98.3%、99.1%、98.6%、98.4%和98.7%,RSD(n=6)分别为0.81%、0.78%、1.1%、1.3%、0.92%和1.1%。结论该方法准确、简便、重复性好,可用于苦参配方颗粒多成分的质量控制。Objective To develop an HPLC-DAD method for the simultaneous determination of 6 alkaloid constitutents（sophoranhol N-oxide, oxymatrine, sophoridine, oxysophocarpine, matrine and sophocarpine） in Kushen dispensing granules. Methods Chromatographic separation was performed on a Waters CSH C18 column（4.6 mm×250 mm, 5 μm） with a 20 mmol·L^（-1） NH4 Ac（0.1% ammonia, p H = 9.0）-[acetonitrilemethanol（1∶1） containing 20 mmol·L^（-1） NH4 Ac] gradient at the flow rate of 0.8 m L·min-1; the detection wavelength was 220 nm, and the column temperature was maintained at 35 ℃. Results Sophoranhol N-oxide, oxymatrine, sophoridine, oxysophocarpine, matrine and sophocarpine were linearity at 0.081-1.620 μg（r= 0.9999）, 0.240-4.800 μg（r = 0.9998）, 0.065-1.300 μg（r = 0.9997）, 0.131-2.620 μg（r = 0.9996）, 0.048-0.950 μg（r = 0.9997）, and 0.045-0.900 μg（r = 0.9998） respectively. The average recoveries were 98.2%, 98.3%, 99.1%, 98.6%, 98.4%, and 98.7%, and the RSDs were 0.81%, 0.78%, 1.1%, 1.3%, 0.92%, and 1.1%, respectively. Conclusion The method is accurate, convenient and reproducible for the quality control of multicomponents in Kushen dispensing granules.

关 键 词：苦参配方颗粒 生物碱 氧化槐醇碱 氧化苦参碱 槐定碱 氧化槐果碱 苦参碱 槐果碱 

分 类 号：R917[医药卫生—药物分析学]