摘要
建立高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定中药材中的伏马毒素B1和B2。样品用甲醇-水(80∶20)溶液提取,经免疫亲和柱净化后,以0.1%甲酸乙腈溶液-0.1%甲酸水溶液为流动相,通过C18色谱柱梯度洗脱,采用电喷雾离子源,正离子模式检测,内标法定量。伏马毒素B1和B2在0.5～500 ng.mL·1内线性关系良好。在4种不同基质5个加样水平的回收率实验中,伏马毒素B1的回收率为84.0%～96.1%,RSD为1.4%～7.6%;伏马毒素B2的回收率为86.3%～99.3%,RSD为1.2%～7.6%。自市售34种中药材样品中,选取10种中药材贮存于高温潮湿的条件中使其发霉,结果在上述发霉样品中有6个呈现阳性结果,其伏马毒素的总含量为82.4～2349μg.kg·1;在24种正常样品中有5种呈现阳性结果,其伏马毒素的总含量为102～729μg.kg·1。本文建立的分析方法灵敏可靠,适用于不同基质中药材中伏马毒素B1和B2的检测。
A rapid and sensitive analytical method was developed for the simultaneous determination of fumonisins B1 and B2 in traditional Chinese medicines by HPLC-MS/MS.The detection limits for fumonisins B1 and B2 were 0.25 ng·mL-1 corresponding to 2 μg·kg-1 in samples.Recoveries from different samples spiked with fumonisins B1 and B2 at levels ranging from 0.2 to 3 mg·kg-1 were 84.0%-96.1% and 86.3%-99.3%,respectively.Among the total of 34 samples purchased from local markets,ten samples of which were visibly moldy samples due to inappropriate storage,and 24 were normal samples.The results showed that 6 of the visibly moldy samples and 5 of the normal samples were contaminated with total fumonisins at levels ranging 82.4-2349 μg·kg-1 and 102-729 μg·kg-1,respectively.
出处
《药学学报》
CAS
CSCD
北大核心
2011年第7期822-827,共6页
Acta Pharmaceutica Sinica
基金
科技部重大新药创制专项(2009ZX09502-025)
国家中医药管理局2008年度中医药行业科研专项(200807042)
