豆芽中30种植物生长调节剂和喹诺酮类药物残留的快速筛查

Rapid Screening of 30 Plant Growth Regulators and Quinolone Antibiotics in Bean Sprout Samples

基于通过型固相萃取净化方法,建立超高效液相色谱-串联质谱(HPLC-MS/MS)法快速筛查豆芽中30种植物生长调节剂和喹诺酮类药物残留的方法。样品以90%乙腈水(含0.1%甲酸)提取,PRiME HLB(新型反相固相萃取小柱)净化,采用Agilent SB-Aq RRHD色谱柱(2.1 mm×100 mm,1.8μm)进行分离,乙腈和0.1%甲酸水溶液为流动相梯度洗脱,采用电喷雾离子源(ESI)在正、负离子多反应监测(MRM)模式下检测,基质加标标准曲线外标法定量。结果显示:30种化合物在2~500μg/L范围内线性良好(r>0.991),方法检出限为0.04~1.67μg/kg,定量限为0.1~5.6μg/kg,平均回收率为74.0%~113.5%,相对标准偏差(RSD)为0.6%~7.7%(n=6)。该方法操作简便,灵敏度高,可对豆芽中30种植物生长调节剂和喹诺酮类药物进行快速筛查。

A method was developed for the simultaneous determination of 30 plant growth regulators residues and quinolone antibiotics residues in bean sprouts by ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with pass-through solid-phase extraction. The samples were extracted by 90% acetonitrile containing 0.1%formic acid and purified with PRiME HLB solid-phase extraction, gradient elution with acetonitrile and water(containing0.1% formic acid). The target compounds were separated on an Agilent SB-Aq RRHD column, then detected by electrospray positive and negative ion multiple reaction monitoring mode. The target compounds were quantified by using the matrix-matched standard calibration. The result showed that the correlation coefficients greater than 0.991 in the range of 2~500 μg/L, the detection limit was 0.04~1.67 μg/kg, the quantitative limit was 0.1~5.6 μg/kg, the average recovery was74.0%~113.5%, and the relative standard deviation was 0.6%~7.7%(n=6). The method is simple and sensitive, can be used for rapid screening of 30 plant growth regulators and quinolones in bean sprouts.