CAJ | 학술논문

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 eV,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/mL,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。
연구료제초제변밀광륭피부접촉오염대중화대섬서분비섬소화학품질적영향。섬소양품경갑순제취,이을정-1％갑산수용액위류동상,액상색보(반상C18주)분리、천련질보( LC-MS/MS)분석검측。질보조건위：MRM모식,탈용제온도500℃,팽당전압30 eV,추공전압위30 V。결과표명,건립적LC-MS/MS측정방법대6충섬서치희표준물질적검출한위0.42~4.86 ng/mL,상관계수R2=0.9953~0.9992,일내화일간RSD위3.8％~6.8％화4.0％~8.8％；가양회수솔위96.9％~109.6％,상대표준편차위2.0％~8.1％。응용차방법검측료36충섬서치희화합물,유20여충화합물자신질보적분면적재변밀광륭오염전후발생개변,변밀광륭피부접촉오염가이개변섬서이후선섬서독소적표체모식。본방법가응용우섬서치희류물질검측。
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.