【摘要】 建立了高效液相色谱-三重四极杆质谱(HPLC-MS/MS)同时测定贝类中22种农药残留的分析方法。样品经含0.1%(v/v)甲酸的乙腈提取,N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化,然后采用ACE UltraCore 2.5 SuperC18柱(100 mm×2.1 mm, 2.5μm)分离,以甲醇-0.1%(v/v)甲酸水溶液为流动相梯度洗脱,流速为0.4 mL/min,柱温为35℃,然后以电喷雾电离(ESI)源,在多反应监测(MRM)、正离子模式下,采用三重四极杆质谱检测。22种农药在各自的线性范围内线性关系良好,相关系数均大于0.997,检出限为0.1～0.3μg/kg,定量限为0.3～1.0μg/kg。在3个添加水平下,22种农药的平均回收率为65.2%～109.4%,相对标准偏差为1.3%～15.2%(n=6)。该方法操作简单,快速,准确度高,灵敏度高,可用于贝类中22种农药残留的同时检测。更多还原

【Abstract】 A method for the simultaneous determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed. The pesticides in the samples were extracted with 0.1%(v/v) formic acid in acetonitrile, cleaned up with primary secondary amine(PSA) and graphitized carbon black(GCB), and then separated on an ACE UltraCore 2.5 SuperC18 column(100 mm×2.1 mm, 2.5 μm) by elution with a methanol-0.1%(v/v) formic acid solution at a flow rate of 0.4 mL/min. The analytes were detected by electrospray ionization in the positive ion mode and the multiple reaction monitoring mode. Good linear relationships were obtained, and the correlation coefficients(r~2) of the 22 pesticides were all higher than 0.997. The limits of detection and limits of quantification were 0.1-0.3 μg/kg and 0.3-1.0 μg/kg, respectively. The mean recoveries varied from 65.2% to 109.4% at three spiked levels, and the relative standard deviations ranged from 1.3% to 15.2%(n=6). The proposed method is simple, accurate, and sensitive, and is effective for the simultaneous determination of 22 pesticide residues detected in shellfish.更多还原