Liu Yongqiang, Liu Sheng, Xu Wenjuan, Tian Guoning, Zhang Jinling
Technical Center for Inspection & Quarantine of Weifang Entry-Exit Inspection & Quarantine Bureau, Weifang 261041, China.
Technical Center for Inspection & Quarantine of Zibo Entry-Exit Inspection & Quarantine Bureau, Zibo 255035, China.
Se Pu. 2017 Sep 8;35(9):941-948. doi: 10.3724/SP.J.1123.2017.06001.
An analytical method was established for the simultaneous determination of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS). The samples were extracted with acetonitrile containing 0.1% (v/v) acetic acid aqueous solution, and cleaned-up by primary secondary amine (PSA) and octadecyl bonded silica (C) adsorbents. The compounds were separated on a Poroshell 120 SB-C column (100 mm×3.0 mm, 2.7 μm) with 0.1% (v/v) formic acid aqueous solution containing 5 mmol/L ammonium acetate-acetonitrile as mobile phases under gradient elution. The eluent was determined by UPLC-Q-TOF/MS with electrospray ionization in positive mode. The quantification analysis was performed with the external standard method. In all ions MS/MS mode, the compounds were qualitatively screened and confirmed by one data acquisition. The correlation coefficients () were greater than 0.995 in the linear ranges of the 44 pesticides. The limits of quantification (LOQs, =10) of the 44 pesticides were 2.5-5.0 μg/kg. At the three spiked levels, the recoveries were between 73.4% and 113.7% with the relative standard deviations (RSDs) ranging from 0.7% to 12.1% (=6). The method effectively improves the determination efficiency of pesticide residues screening by high-resolution mass spectrometry.
建立了超高效液相色谱-四极杆-飞行时间质谱联用(UPLC-Q-TOF/MS)同时测定生姜和大葱中44种农药残留的分析方法。样品用含0.1%(v/v)乙酸的乙腈水溶液提取,并用伯仲胺(PSA)和十八烷基键合硅胶(C18)吸附剂净化。采用Poroshell 120 SB-C18色谱柱(100 mm×3.0 mm,2.7 μm),以含5 mmol/L乙酸铵的0.1%(v/v)甲酸水溶液-乙腈为流动相进行梯度洗脱分离化合物。采用电喷雾电离正模式的UPLC-Q-TOF/MS测定洗脱液。采用外标法进行定量分析。在全离子MS/MS模式下,通过一次数据采集对化合物进行定性筛选和确证。44种农药在其线性范围内的相关系数(r)均大于0.995。44种农药的定量限(LOQs,n = 10)为2.5~5.0 μg/kg。在3个加标水平下,回收率在73.4%~113.7%之间,相对标准偏差(RSDs)为0.7%~12.1%(n = 6)。该方法有效提高了高分辨质谱筛查农药残留的测定效率。