分析化学Issue(9)：1415-1421,7.DOI:10.11895/j.issn.0253-3820.150038
四级杆串联质谱分析苄嘧磺隆污染蟾蜍耳后腺中蟾蜍甾烯水平
Effect of Bensulfuron Pollution on Levels of Bufadienolides from Venom Secreted by Toad
摘要
Abstract
Ulta performance liqiuid chromatography-triple quadrupole tandem mass spectrometry ( UPLC-MS/MS) was used to monitor the relative levels of bufadienolides in toad venom in normal and bensulfuron-polluted groups. Methanol extract of toad venom was separated by UPLC ( ODS-C18 ) using a gradient elution of water contains 0. 1% formic acid and acetonitrile. Mass spectrometry was used in an ESI source operated in positive ion and MRM mode. The parameters in the source were set as follows: capillary voltage 3. 0 kV; sampling cone voltage 30 V; and desolvation temperature 500℃. In this method, external calibrations of 6 standards were typically constructed (R2=0. 9953-0. 9992). The LOD was 0. 42-4. 86 ng/mL. Intra- and inter-day precision was 3. 8%-6. 8% and 4. 0%-8. 8%, respectively. The recovery of standard was evaluated by spiking the standard compound into toad venom. Their average recoveries were 96. 9%-109. 6%, and RSDs were 2. 0%-8. 1%. This method was further employed into monitoring the levels of 36 bufadienolides. The levels of more than 20 bufadienolides were greatly different after bensulfuron pollution, suggesting that the bensulfuron pollution could change the chemical expression pattern of bufadienolides in toad venom.关键词
中药资源学/蟾蜍/苄嘧磺隆/蟾酥Key words
Chinese resources/Toad/Bensulfuron/Venenum Bufonis引用本文复制引用
周婧,王洪兰,马宏跃,闫文丽,龚艳,钱琎,段金廒,吴启南..四级杆串联质谱分析苄嘧磺隆污染蟾蜍耳后腺中蟾蜍甾烯水平[J].分析化学,2015,(9):1415-1421,7.基金项目
本文系国家自然科学青年基金(Nos.81102762,3901894,81274199),江苏省中药资源产业化过程协同创新中心基金(No. ZDXM-1-14),江苏省六大人才高峰C类(No. YY-015),江苏高校优势学科建设工程资助项目(No. PAPD)资助This work was supported by the National Natural Science Foundation of China (Nos.81102762,3901894,81274199) （Nos.81102762,3901894,81274199）
