QuEChERS结合柱净化的超高效液相色谱-串联质谱法测定有机肥中46种抗生素

发布时间：2018-05-05 03:06

本文选题：超高效液相色谱-串联质谱法(UPLC-MS/MS) + 抗生素残留　；参考：《分析测试学报》2017年02期

【摘要】：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定有机肥中磺胺类、喹诺酮类、大环内酯类46种抗生素的分析方法。样品用乙腈-EDTA缓冲溶液(p H 10.0)提取,盐析后离心分层,乙腈层按Qu ECh ERS法,采用吸附剂净化;缓冲溶液层经HLB柱净化。ACQUITY UPLC BEH C18柱用作色谱分离,以2mmol/L甲酸铵水溶液(含0.1%甲酸)-甲醇为流动相进行梯度洗脱;电喷雾电离源正离子(ESI+)多反应监测(MRM)模式检测,基质外标法定量。46种抗生素在1~200μg/L范围内线性关系良好,相关系数(r2)为0.996 6~0.999 9。在25,100,400μg/kg加标浓度下,3类抗生素的回收率分别为67.8%~95.6%,65.6%~89.4%和66.6%~107.8%,相对标准偏差为0.4%~11.9%;方法检出限(S/N=3)为0.6~4.6μg/kg,定量下限(S/N=10)为2.1~15.4μg/kg。
[Abstract]:A method for the simultaneous determination of sulfonamides, quinolones and macrolides in organic fertilizers by UPLC-MS / MS was established. The sample was extracted by acetonitrile-EDTA buffer solution (pH 10.0), separated by centrifugation after salting out, purified by adsorbent in acetonitrile layer according to Qu ECh ERS method, and purified by HLB column. ACQUITY UPLC BEH C18 column was used as chromatographic separation. Using 2mmol/L ammonium formate aqueous solution (containing 0.1% formate-methanol as mobile phase for gradient elution, and electrospray ionization source (ESI) for multi-reaction monitoring), the matrix external standard method was used to determine the linear relationship between the quantification of .46 antibiotics in the range of 1 ~ 200 渭 g / L, and in the range of 1 ~ 200 渭 g / L. The correlation coefficient (r _ 2) is 0.996 ~ 0.999 ~ 9. At the concentration of 25100400 渭 g/kg, the recoveries of the three antibiotics were 67.8% and 65.6%, 89.4% and 66.6%, respectively, and the relative standard deviation was 0.4 渭 g / kg, and the detection limit was 0.6 渭 g / kg, and the lower limit was 2.1 渭 g / kg and 15.4 渭 g / kg / kg, respectively.
【作者单位】：浙江省农业科学院农产品质量标准研究所浙江省植物有害生物防控重点实验室-省部共建国家重点实验室培育基地;浙江工业大学化工学院;浙江医药股份有限公司;
【基金】：农业部公益性行业专项(201303091) 浙江省自然科学基金(LY14B070008) 省部共建国家重点实验室培育基地项目(2010DS700124-ZZ1602) 浙江省农业科学院中美三方合作项目(2010DS700124-ZM1604) 宁波科技项目(2013C11024)
【分类号】：TQ440.72;O657.63

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