目的：应用超高效液相色谱-电喷雾串联四极杆质谱联用技术,建立动物组织中20种β2-兴奋剂残留的多组分检测方法。方法：样品经酶解、高氯酸沉淀蛋白,MCX柱净化和富集。选择沙丁醇胺-d3,克伦特罗-d9,莱卡多巴胺-d9为内标,通过Waters ACQUITY UPLCTMBEHShield RP C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相,梯度洗脱,MRM方式测定。结果：该方法的检出限为0.01-0.33μg/kg,最低定量限为0.04-1.11μg/kg。添加水平为0.5、1.0、2.0μg/kg时,20种β2-兴奋剂的加标回收率为75.5%-108.4%,相对标准偏差为2.9%-19.0%。结论：该方法灵敏度高、回收率好,能够快速准确地对动物组织中20种β2-兴奋剂进行检测。
This article presents the designing and fabrication of a microfluoidic chip with an integrated supported-liquid-membrane extraction-back-extraction and chip-based capillary electrophoresis system(SLMEBE-CCE).A 3-dimensional channel network for the SLMEBE-CCE system was fabricated with a four-layer glass/PTFE-membrane hybrid structure. With a gravity pump for sample and back-extraction solution delivery and a multi-channel high-voltage supply for CCE separation,the microchip with the coupled SLMEBE-CCE system was demonstrated by the pre-concentration,separation and detection of a mixed solution of fluorescein and butyl-rhodamine B.Compared to chip-based CCE without SLMEBE,the developed SLMEBE-CCE system produced a 7-fold increase in the signal of the model analyte of fluorescein and a 4-fold decrease in the signal of the model co-existing compound of butyl-rhodamine B.
目的建立超高效液相色谱-串联质谱法同时检测消毒卫生产品中的5种硝基咪唑类抗生素和17种磺胺类抗生素。方法样品加入混合内标溶液后,经2%甲酸水溶液和乙腈混合溶剂(3∶2,V/V)超声提取,上清液经2%甲酸水溶液稀释后,经MCX固相萃取柱富集净化,2%甲酸水溶液和甲醇溶液分别淋洗,5%氨水甲醇洗脱,洗脱液经氮吹至近干后,1.0 mL 10%甲醇水溶液复溶,经CORTECS^(TM) UPLC C_(18)(100 mm×2.1 mm, 1.6μm)反相色谱柱分离,超高效液相色谱-串联质谱仪检测分析。结果 22种抗生素在0.05～5.0 ng/mL范围内线性关系良好,相关系数均大于0.999;方法的检出限为0.03～0.15μg/kg,加标回收率为84.3%～121.2%,相对标准偏差为1.13%～8.43%(n=6)。该方法成功用于20份膏霜、水剂型抗(抑)菌消毒产品中违禁抗生素的检测,阳性检出率为45%。结论该方法灵敏度高、选择性好、操作简单,适用于膏霜、水剂型消毒产品中违禁抗生素的检测。
