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

作　　者：周婧[1] 王洪兰[1] 马宏跃[1] 闫文丽[1] 龚艳[1] 钱琎[1] 段金廒[1] 吴启南[1] 

机构地区：[1]南京中医药大学药学院江苏省中药资源产业化协同创新中心,南京210023

出　　处：《分析化学》2015年第9期1415-1421,共7页Chinese Journal of Analytical Chemistry

基　　金：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~~

摘　　要：研究了除草剂苄嘧磺隆皮肤接触污染对中华大蟾蜍分泌蟾酥化学品质的影响。蟾酥样品经甲醇提取,以乙腈-1%甲酸水溶液为流动相,液相色谱（反相C18柱）分离、串联质谱（LC-MS/MS）分析检测。质谱条件为：MRM模式,脱溶剂温度500℃,碰撞电压30 e V,锥孔电压为30 V。结果表明,建立的LC-MS/MS测定方法对6种蟾蜍甾烯标准物质的检出限为0.42~4.86 ng/m L,相关系数R2=0.9953~0.9992,日内和日间RSD为3.8%~6.8%和4.0%~8.8%;加样回收率为96.9%~109.6%,相对标准偏差为2.0%~8.1%。应用此方法检测了36种蟾蜍甾烯化合物,有20余种化合物自身质谱积分面积在苄嘧磺隆污染前后发生改变,苄嘧磺隆皮肤接触污染可以改变蟾蜍耳后腺蟾蜍毒素的表达模式。本方法可应用于蟾蜍甾烯类物质检测。Uha 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 

分 类 号：S858.9[农业科学—临床兽医学]