芽苗类蔬菜中喹诺酮类药物的高效液相色谱-质谱测定法  

Determination of Quinolones Residues in Shoots by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：吴淑秀 公茂金 刘玉芳 朱万燕 刘冰 刘金峰 

机构地区：[1]临沂出入境检验检疫局检验检疫技术中心,山东临沂276034 [2]山东省交通技术学院

出　　处：《环境与健康杂志》2012年第5期457-459,共3页Journal of Environment and Health

摘　　要：目的建立了芽苗类蔬菜中喹诺酮类药物的分散固相萃取-高效液相色谱(HPLC)-质谱(MS-MS)检测方法。方法样品经酸化乙腈均质提取,使用100mg乙二胺-N-丙基硅烷(PSA)基质分散净化剂净化。选择甲醇+乙腈(体积比为40:60)和0.2%甲酸溶液作为流动相,进行梯度洗脱。采用HPLC-MS-MS进行检测。为消除样品基质效应,以空白样品提````取液作为标准溶液的稀释溶液。结果在1～100μg/L线性范围内,四种喹诺酮类药物的回归方程均呈较好的线性关系,r≥0.99。该方法的检出限为0.06～0.25μg/kg,定量下限为0.22～0.84μg/kg,平均回收率在74.10%～93.66%之间,RSD在2.0%～6.3%之间。结论该方法操作简单、快速、准确,适用于芽苗类蔬菜中喹诺酮类药物残留的检验。Objective To establish a method for the determination of quinolones residues in shoots. Methods The analytes were extracted from the samples using acedified acetonitrile, and purified by matrix solid-phase dispersion（MSPD） using PSA as solidphase, then analyzed by LC-MS-MS with multiple-reaction monitoring （MRM）. The interference of matrix was reduced by the matrix-matched calibration standards curve. Results The linear range was 1-100 μg/L for four quinolones with good correlation coefficients （r≥0.99）, the limits of detection were 0.06-0.25 μg/kg, and the limits of quantification were 0.22-0.84 μg/kg for four quinolones. The average rates of recovery were 74.10%-93.66% , the RSDs were 2.0%-6.3%. Conclusion This method is simple, rapid, accurate and applicable to the determination of quinolones in shoots.

关 键 词：色谱法 液相 串联质谱 芽苗 喹诺酮类 残留 

分 类 号：O657.6[理学—分析化学]