摘要
目的:建立一种快速灵敏的同时测定桂林西瓜霜喷剂(西瓜霜,黄连,黄芩等)中的有效成分苦参碱、小檗碱、黄芩苷和靛玉红的液相色谱/质谱(HPLC/MS)方法。方法:采用Zorbax SB C18(3.0mm×250mm,5μm)色谱柱,以含0.5%甲酸的水(A)-甲醇(B)体系为流动相进行线性梯度洗脱,梯度洗脱程序为:0—2min,60%B;2~5min,60%-90%B;5min至结束,90%B;流速:0.40mL/min;在ESI正离子模式下,采用选择性离子监测方法:0—3min,m/z249;3—6min,m/z336;6~10min,m/z447;10~16min,m/z263。苦参碱在0.020—10μg/mL,小檗碱在0.010~40.0μg/mL,黄芩苷在0.036~50.0μg/mL,靛玉红在0.040~4.00μg/mL范围内峰面积与浓度呈良好的线性关系;检出限分别为0.005,0.001,0.006,0.010μg/mL。4种成分的加样回收率均在96%~101%之间,相对标准偏差RSD小于3%。结论:方法快捷,准确,重现性好。可为桂林西瓜霜喷剂的质量控制提供参考依据。
AIM : To establish an HPLC-MS method for simultaneously determining four effective components in Guilin Watermelon Frost ( Mirabilitum Praeparatum, Rhizoma Coptidis, Radix Scutellariae, etc. ). METHODS : The sample was extracted with methanol containing 20% chloroform under ultrasonication. The HPLC separation was performed on Zorbax SB Cls (3.0 mm ×250 mm, 5 μm) column using water including 0.5% formic acid (A)-methanol (B) as mobile phase, with the gradient elution (0-2 min, 60% B; 2-5 min, 60%±90% B; 5 rain to the end, 90%B), at a flow rate of 0.40 mL/min. The compounds were analyzed by ESI-MS under ion monito- ring mode(0-3 min, m/z 249; 3-6 min, m/z 336; 6-10 min, m/z447; 10-16 min, m/z 263). RESULTS: The linear ranges were 0. 020-10.0 μg/mL, 0. 010-40.0 μg/mL, 0. 036-50.0 μg/mL and 0. 040-4.00 μg/mL for matrine, berberine, baicalin and indirubin, with detection limits of 0. 005, 0.001, 0. 006 and 0. 010 μg/mL, respectively. The average recoveries ranged from 96% to 101% with all relative standard deviations less than 3%.CONCLUSION: The method is rapid, accurate and suitable for the quality control of the four effective components in Guilin Watermelon Frost.
出处
《中成药》
CAS
CSCD
北大核心
2009年第1期68-71,共4页
Chinese Traditional Patent Medicine
基金
广西自然科学基金资助项目(桂科自0832034)