超高效液相色谱-串联质谱法同时测定草莓和杨梅中35种杀菌剂残留

Simultaneous determination of 35 fungicide residues in strawberry and Chinese bayberry( myrica rubra) by ultra-performance liquid chromatography-tandem mass spectrometry

目的建立一种超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定草莓和杨梅中35种杀菌剂残留量的分析方法。方法用乙腈提取试样中的杀菌剂残留,提取液浓缩后,经氨基固相萃取小柱净化,以Phenomenex XB-C18(100 mm×2.1 mm,2.6μm)为色谱柱,以甲醇和5 mmol/L乙酸铵-0.1%乙酸缓冲溶液为流动相进行梯度洗脱,在多反应监测(MRM)模式下测定,基质匹配标准溶液外标法定量。结果 35种杀菌剂得到良好的分离,方法的线性范围为2μg/L^1 000μg/L,检出限(S/N=3)为0.03μg/kg^1.16μg/kg,定量限(S/N=10)为0.12μg/kg^3.88μg/kg。在10μg/kg的添加水平下,回收率为62.61%~130.53%,相对标准偏差为2.1%~9.5%。结论实验结果表明,该方法操作简便,耗时短,提取效果好,灵敏度高,准确性和稳定性好,应用于日常检测可大大降低检测成本,缩短检测周期,具有实际应用价值。

Objective To establish a method for simultaneous determination of 35 fungicides in strawberry and Chinese bayberry （ Myrica rubra） by UPLC - MS/MS. Methods The fungicide residues were extracted from the samples by acetonitrile, cleaned - up with an amino SPE column and then analyzed using UPLC - MS/MS in multiple reaction monitoring （MRM） mode with posi- tive electrospray ionization. The chromatographic analysis was carried out on a Phenomenex XB - C18 （ 100 mm×2. 1 mm, 2.6μm） column with methanol and 5 mmol/L ammonium acetate buffer solution （contain 0.1% acetic acid） as the mobile phases in gradient program, and quantified by matrix - matched external standard method. Results 35 fungicides Were well separated. The linear range of the calibration curve was 2 μg/L - 1 000 μg/L, The limits of quantification （ S/N = 10） of the 35 fungicides were 0.12 μg/kg - 3.88μg/kg and the limits of detection （ S/N = 3 ） were 0.03 μg/kg - 1.16 μg/kg. The re- coveries of the fungicides spiked in strawberry and bayberry samples were 62.61% - 130.53% at the spiked levels of 10μg/kg. The relative standard deviations （RSDs） were 2.1% -9.5%. Conclusion The method is simple, time - saving and environmental friendly with high sensitivity and good reproducibility, as well as having practical application value for its low - cost and short - circle.