超高效液相色谱_串联质谱法测定鱼组织中的6种抗雌激素药物.docxVIP

研究论文DOI: 10． 3724 / SP． J ． 1123． 2011． 01055摘要: 采用超高效液相色谱-串联质谱( UPLC-MS / MS) 在多反应监测( MRM ) 模式下建立了鱼肉、鱼肝中 6 种抗雌激素类药物( 托瑞米芬、氯米芬、他莫昔芬、雷洛昔芬、阿那曲唑、来曲唑) 的检测方法。样品采用乙腈超声提取，上 清液中加入适量水稀释提取液，经混合型阳离子交换( MCX) 固相萃取柱富集、净化后进行 UPLC-MS / MS 分析。 UPLC 分离在 ACQUITY UPLC TM BEH C18 柱( 100 m m × 2. 1 m m ，1. 7 μm ) 上进行，以乙腈和 0. 1% 甲酸水溶液为 流动相进行梯度洗脱。6 种抗雌激素药物的定量限( 以信噪比为 10 计) 为 0. 1 ～ 0. 3 μg / kg ; 4 个加标水平的平均 回收率为 84. 9% ～ 112. 2%，相对标准偏差为 0. 9% ～ 14. 3%。该方法可用于鱼肉、鱼肝中 6 种抗雌激素药物的痕量 分析。关键词: 固相萃取; 超高效液相色谱-串联质谱; 抗雌激素药物; 鱼肉; 鱼肝中图分类号: O658文献标识码: A文章编号: 1000-8713( 2011) 11-1055-07Abstract: A co m prehensive analytical m etho d based o n ultra perfo rm ance liquid chro m ato gra-phy -tandem m ass spectro m etry ( UPLC -MS / MS ) has been develo ped fo r the sim ultaneo us determ inatio n o f 6 antiestro gens ( to rem ifene ，clo m iphene ，tam o x ifen ，ralo x ifene ，anastro zo le and letro zo le ) in fish m uscle and liver． The m ulti-reactio n m o nito ring m o de w as em plo yed fo r the determ inatio n ． The ho m o geneo us fish tissue sam ples w ere ultraso nically ex tracted w ith ace- to nitrile ，and then the supernatants w ere diluted by w ater． The target co m po unds w ere co ncen- trated and purified by a m ix ed -m o de catio nic -ex changer ( MCX) cartridge ，and then separatedo n an ACQUITY UPLC TM BEH C18 co lum n ( 100 m m × 2. 1 m m ，1. 7 μm )using a binary m o bilephase gradient w ith w ater co ntaining 0. 1% fo rm ic acid and aceto nitrile ． The lim its o f quantifi-catio n ( LOQ ，S / N = 10)o f the 6 antiestro gens w ere 0. 1 － 0. 3 μg / kg in m uscle and liver sam -ples ． The average reco veries o f target co m po unds ( spiked at fo ur co ncentratio n levels ) basedo n internal standard calibratio n w ere in the range o f 84. 9% － 112. 2% w ith the relative standard deviatio ns o f 0. 9% － 14. 3%． This m etho d can be applied to the trace analysis o f target drugs in fish m uscle and liver sam ples ．Key words: so lid phase ex tractio n ( SPE ) ; ultra