摘要
建立了以固相萃取-液相色谱-电喷雾质谱（SPE—LC—ESI／MS）法检测蘑菇中咪鲜安残留量的方法。蘑菇样品加入乙腈萃取，离心分离，取上清液加入NaCl和MgSO4进行盐析，有机相浓缩后加入键合丙基乙二胺（PSA）净化，上清液以0．45μm针头过滤器过滤后进样。色谱柱为ZORBAX Eclipse XDB-C18（150×2．1mm，3．5μm）柱，柱温40℃；流动相为0．1％乙酸水溶液-乙腈（30＋70，V／V），流速0．20mL／min。质谱采用选择离子监控模式，检测离子的质荷比（m/z）分别为380、378、376、312、310和308。咪鲜安在样品中的加标回收率为95．00％～100．07％，变异系数在1．72％～8．71％之间，检出限（S／N〉10）为2．86μg／L。此方法简单，准确，将其应用于蘑菇中咪鲜安的消解动态研究，取得了比较理想的效果。
In this paper, solid-phase extraction （SPE） combined with high performance liquid chromatography （LC）/electrospary ionization mass spectrometry （ESI/MS） was used to detect the residue of prochloraz, an ergosterol biosynthesis inhibiting fungicide, in mushroom. Samples were extracted from mushroom with acetonitrile, then the extracts were salted out with NaCl and MgSO4. Supernatant was concentrated with gas and cleaning-up with SPE. After filtrating with 0. 45 μm millipore filter, the solution was detected by LC-MS. Optimized conditions involved separation on a ZORBAX Eclipse XDB-C18 column（150×2.1 mm,3.5 μm） at 40℃, acetonitrile and 0.1% acetic acid （70＋ 30, V/V）at 0. 2 mL/min as mobile phase. The analysis was performed in the selected ion monitoring（SIM） mode with m/z380,378,376,312,310 and 308. The fortified recovery of prochloraz ranged from 95.0% to 100.1%, with coefficient of variance（CV）in the region of 1.72%-8.71%. The limit of detection was 2.86μg/L （S/N〉10）. The developed method is accurate and has been applied to the investigation of the degradation of prochloraz 50% WP in mushroom with satisfactory results.
出处
《分析科学学报》
CAS
CSCD
2007年第5期523-526,共4页
Journal of Analytical Science
关键词
液相色谱-质谱
咪鲜安
蘑菇
残留检测
Liquid chromatography / electrospary ionization mass spectrometry
Prochloraz
Mushroom
Residue detection
