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超高效液相色谱-串联质谱法同时测定罗非鱼养殖淡水中的9种喹诺酮类药物含量
引用本文:吴学贵,王一晨,陈少莉,黄肖凤,李小梅,王芳姑. 超高效液相色谱-串联质谱法同时测定罗非鱼养殖淡水中的9种喹诺酮类药物含量[J]. 食品安全质量检测学报, 2019, 10(19): 6561-6567
作者姓名:吴学贵  王一晨  陈少莉  黄肖凤  李小梅  王芳姑
作者单位:海南威尔检测技术有限公司
摘    要:目的建立超高效液相色谱-串联质谱联用法(ultraperformanceliquidchromatography-tandemmass spectrometry, UPLC-MS/MS)测定罗非鱼养殖淡水中9种喹诺酮类药物的分析方法。方法探究优化色谱条件、固相萃取柱条件、洗脱液比例和体积等对回收率产生影响的主要因素。样液制成0.1 mol/L Na2EDTA-Mcllvaine缓冲溶液后调节pH为4.0、采用聚合物固相萃取柱进行净化,吹干浓缩、溶解过滤后,经乙腈和乙酸铵-甲酸水溶液梯度洗脱、色谱柱Poroshell 120 EC-C18(50 mm×2.1 mm, 2.7μm)分离、超高效液相色谱-串联质谱仪测定, 8种化合物内标法定量, 1种化合物外标法定量。结果 9种目标物的检出限为0.02~0.2 ng/L,平均回收率为80.1%~110.3%,相对标准偏差(relative standard deviation, RSD)均小于10%。结论本方法经济、简便、稳定、准确性高,能满足实际罗非鱼养殖淡水中9种喹诺酮类药物含量测定的要求。

关 键 词:超高效液相色谱-串联质谱法   养殖淡水   喹诺酮   内标法   外标法
收稿时间:2019-08-08
修稿时间:2019-10-08

Simultaneous determination of 9 kinds of quinolones in tilapia cultured fresh water by ultra performance liquid chromatography-tandem mass spectrometry
WU Xue-Gui,WANG Yi-Chen,CHEN Shao-Li,HUANG Xiao-Feng,LI Xiao-Mei and WANG Fang-Gu. Simultaneous determination of 9 kinds of quinolones in tilapia cultured fresh water by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2019, 10(19): 6561-6567
Authors:WU Xue-Gui  WANG Yi-Chen  CHEN Shao-Li  HUANG Xiao-Feng  LI Xiao-Mei  WANG Fang-Gu
Affiliation:Hainan Willtest Technology Co., Ltd,Hainan Willtest Technology Co., Ltd,Hainan Willtest Technology Co., Ltd,Hainan Willtest Technology Co., Ltd,Hainan Willtest Technology Co., Ltd and Hainan Willtest Technology Co., Ltd
Abstract:Objective To establish a method for the determination of 9 kinds of quinolones in tilapia cultured fresh water by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The main factors influencing the recovery were optimized, such as chromatographic conditions, solid-phase extraction column conditions, eluent ratio and volume optimization. The sample liquid made from 0.1 mol/L Na2EDTA- Mcllvaine buffer solution, was purified by polymer solid phase extraction column after adjusting the pH to 4.0, blow dry enrichment dissolved after filtering, then the sample was separated on chromatography column Poroshell 120 EC-C18 (50 mm to 2.1 mm, 2.7 microns) after gradient elution with acetonitrile and ammonium acetate-formic acid aqueous solution, and determined by UPLC-MS/MS. Eight compounds were quantified by internal standard method and one compound was quantified by external standard method. Results The limits of detection of the 9 targets were 0.02?0.2 ng/L, the average recoveries were 80.1%?110.3%, and the relative standard deviations were less than 10%. Conclusion This method is economical, simple, stable and accurate, and can meet the requirements of the determination of 9 quinolones in tilapia cultured fresh water.
Keywords:ultra performance liquid chromatography-tandem mass spectrometry   cultured fresh water   quinolones   internal standard method   external standard method
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