摘要
建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)同时检测水产及水产加工品中24种镇静剂类药物的分析方法。样品经乙腈提取,浓缩近干后,用50%(v/v)甲醇水溶液定容,再用乙腈饱和的正己烷溶液净化。采用ACQUITY UPLC~BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)分离,以0.1%(v/v)甲酸水溶液和含0.1%(v/v)甲酸的乙腈溶液为流动相进行梯度洗脱,在可加热电喷雾离子(HESI)源正离子模式和全扫描/数据依赖二级扫描(Full MS/dd-MS^2,Top1)模式下检测,外标法定量。结果表明,24种镇静剂在各自的范围内线性关系良好,决定系数(r^2)≥0.996 8;在6种水产及水产加工品基质中进行3个不同添加水平的加标回收试验,24种镇静剂类药物的平均回收率为58.9%~122.9%,相对标准偏差为0.1%~16.4%(n=6);24种镇静剂类药物的定量限为0.1~5.0μg/kg。该法操作简便,精密度高,准确性好,适用于批量水产及水产加工品中24种镇静剂类药物的快速筛查。
A method was developed for the simultaneous determination of 24 tranquillizer drugs in fish and fishery products using ultra-high performance liquid chromatography- quadrupole/ electrostatic field orbitrap high resolution mass spectrometry （UPLC-Q-Orbitrap HRMS）. The samples were extracted with acetonitrile. Then,the extracts were concentrated,dissolved by 50% （v/v ） methanol aqueous solution,cleaned up with hexane saturated by acetonitrile. The separation was performed on an ACQUITY UPLC？ BEH C18 column （100 mm x 2. 1 mm,1.7 pm） with the gradient elution using acetonitrile and water both containing 0. 1% （v/v ） formic acid as mobile phases. The drugs were analyzed by full MS scan/data dependent MS2（ Full MS/dd-MS2） （Top 1） mode by heating electrospray ion （HESI） source. The results were quantified by external standard method. The calibration curves of the 24 tranquillizer drugs were linear in their respective linear range, the decision coefficients （r2） were no less than 0. 996 8. The aver-age spiked recoveries of the 24 tranquillizer drugs were 58. 9 % -122. 9 % , and the relative stand-ard deviations （RSDs） were 0. 1% -16. 4 % in the six kinds of fish and fishery products at three spiked levels. The limits of quantification （LOQs） of the 24 tranquillizer drugs were 0. 1-5.0 pg/kg. The method is simple, rapid, sensitive,reliable and suitable for the screening of the 24 tranquillizer drugs in fish and fishery products.
出处
《色谱》
CAS
CSCD
北大核心
2018年第2期125-135,共11页
Chinese Journal of Chromatography
基金
广东省省级科技计划项目(2015A050502010
2014A040401011)
中山市社会公益重大专项(2015B2295)~~
关键词
超高效液相色谱
四极杆/静电场轨道阱高分辨质谱
镇静剂类药物
水产及水产加工品
ultra-high performance liquid chromatography （UPLC）
quadrupole/electrostatic field orbitrap high resolution mass spectroscopy （Q-Orbitrap HRMS）
tranquillizer drugs
fish and fishery products
