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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 dispersive solid phase extraction-high performance liquid chromatography-mass spectrometry (MS-MS) method for the determination of quinolones in sprouted vegetables. Methods Samples were homogenized with acidified acetonitrile and purified using 100 mg of ethylenediamine-N-propylsilane (PSA) matrix-dispersed cleaning agent. Methanol + acetonitrile (40:60 by volume) and 0.2% formic acid solution were selected as the mobile phase and gradient elution was carried out. Using HPLC-MS-MS detection. In order to eliminate the matrix effect of the sample, a blank sample is used to take a solution as a dilute solution of the standard solution. Results The regression equation of four quinolones showed a good linear relationship in the linear range of 1 ~ 100μg / L, r≥0.99. The detection limit of the method was 0.06 ~ 0.25μg / kg, the lower limit of quantification was 0.22 ~ 0.84μg / kg, the average recovery was between 74.10% ~ 93.66%, RSD was between 2.0% ~ 6.3%. Conclusion The method is simple, rapid and accurate and is suitable for the determination of quinolone residues in sprouts and vegetables.