石墨化多壁碳纳米管复合净化-高效液相色谱-串联质谱法测定植物源性食品中乙氧呋草黄残留量
HPLC-MS/MS Determination of Residual Amount of Ethofumesate in Vegetative Food with Graphitized MWNTs Composite Purification
-
摘要: 植物源性食品样品先后用正己烷和50%（体积分数）乙腈溶液分别提取，经3种吸附剂石墨化多壁碳纳米管（MWNTs）、强阴离子交换机理的硅胶（SAX）和N-丙基乙二胺（PSA）复合净化，上清液过滤后采用高效液相色谱-串联质谱法测定滤液中乙氧呋草黄残留量。以JADE-PAK CB-C18色谱柱为固定相，以不同体积比的0.1%（体积分数）甲酸溶液和乙腈的混合液为流动相进行梯度洗脱，串联质谱分析中采用电喷雾离子源正离子模式和多反应监测模式。乙氧呋草黄在不同基质中的线性范围均为20~100 μg·L-1，检出限（3S/N）为6.0 μg·kg-1，测定下限（10S/N）为20.0 μg·kg-1。以空白样品为基体进行加标回收试验，所得回收率为74.1%~121%，测定值的相对标准偏差（n=6）为2.8%~16%。Abstract: The vegetative food sample was extracted with hexane and 50% (φ) acetonitrile solution respectively. After composite purification by 3 adsorbents (graphitized MWNTs, SAX and PSA), the supernatant was taken and filtered. HPLC-MS/MS was applied to the determination of residual amount of ethofumesate in the filtrate. JADE-PAK CB-C18 chromatographic column was used as stationary phase, and the mixture of 0.1% (φ) formic acid solution and acetonitrile mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linearity ranges of ethofumesate in various matrices were all found between 20 μg·L-1 and 100 μg·L-1, with detection limits (3S/N) of 6.0 μg·kg-1 and lower limits of determination (10S/N) of 20.0 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 74.1%-121%, with RSDs (n=6) of determined values in the range of 2.8%-16%.WT5HZ
下载: