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.
出处
《环境与健康杂志》
CAS
CSCD
北大核心
2012年第5期457-459,共3页
Journal of Environment and Health
关键词
色谱法
液相
串联质谱
芽苗
喹诺酮类
残留
Chromatography, liquid
Tandam mass
Shoots
Quinolones
Residue