QuEChERS-超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速测定水产品中25种药物残留
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摘要
采用了一种高效基质脂肪吸附剂(EMR-Lipid)去除水产品基质中的脂肪和磷脂等杂质,利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UPLC-Q Orbitrap HRMS)的同时定性定量功能,建立了水产品中25种药物残留的检测方法。样品经乙腈提取,EMR-Lipid净化,同时加入3 g氯化钠和3 g无水硫酸钠进行盐析,采用ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,以含0.1%(v/v)甲酸的乙腈溶液和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,在加热电喷雾离子(HESI)源、全扫描/实时二级质谱扫描(Full MS/ddMS2)监测模式下进行检测。结果表明,25种目标化合物的质量浓度与母离子峰面积间的线性关系良好,相关系数(r)均大于0.997;25种目标化合物的检出限为0.1~1.0μg/kg,其平均加标回收率为70.1%~108.9%,相对标准偏差为2.1%~13.8%。该法具有操作简单快捷、灵敏度高等优点。
An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q Orbitrap HRMS)method was developed for the rapid screening of 25 drug residues in aquatic products by the application of a novel enhanced matrix removal of lipids(EMR-Lipid). The samples were extracted with acetonitrile,cleanedup with EMR-Lipid,and salted out with 3. 0 g sodium chloride and 3. 0 g sodium sulfate. Theseparation of the 25 drug residues was performed on an ACQUITY UPLC BEH C18 column(100 mm×2. 1 mm,1. 7 μm)with gradient elution. Acetonitrile containing 0. 1%(v/v)formic acid and 0. 1%(v/v)formic acid aqueous solution were used as mobile phases. The compounds were detected by Full scan/date dependent MS/MS(Full MS/dd-MS2)via heated electrospray ionization(HESI)source. The calibration curves were linear with correlation coefficients(r)greater than 0. 997. The limits of detection(LODs)ranged from 0. 1 μg/kg to 1. 0 μg/kg. The average spiked recoveries of the 25 target compounds were between 70. 1% and 108. 9% with relative standard derivations(RSDs)from 2. 1% to 13. 8%. Compared with the previous methods,this method has characteristics of simpler sample preparation and higher sensitivity.
An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q Orbitrap HRMS)method was developed for the rapid screening of 25 drug residues in aquatic products by the application of a novel enhanced matrix removal of lipids(EMR-Lipid). The samples were extracted with acetonitrile,cleanedup with EMR-Lipid,and salted out with 3. 0 g sodium chloride and 3. 0 g sodium sulfate. Theseparation of the 25 drug residues was performed on an ACQUITY UPLC BEH C18 column(100 mm×2. 1 mm,1. 7 μm)with gradient elution. Acetonitrile containing 0. 1%(v/v)formic acid and 0. 1%(v/v)formic acid aqueous solution were used as mobile phases. The compounds were detected by Full scan/date dependent MS/MS(Full MS/dd-MS2)via heated electrospray ionization(HESI)source. The calibration curves were linear with correlation coefficients(r)greater than 0. 997. The limits of detection(LODs)ranged from 0. 1 μg/kg to 1. 0 μg/kg. The average spiked recoveries of the 25 target compounds were between 70. 1% and 108. 9% with relative standard derivations(RSDs)from 2. 1% to 13. 8%. Compared with the previous methods,this method has characteristics of simpler sample preparation and higher sensitivity.
引文
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[16]Jia W,Chu X G,Ling Y,et al.J Chromatogr A,2014,1347:122
[17]Solliec M,Roy-Lachapelle A,Sauve S.Anal Chim Acta,2015,853:415
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