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该文采用Qu ECh ERS方法提取净化烟草样品,建立了超高效液相色谱-串联质谱(UPLC-MS/MS)检测烟草中腈菌唑的残留分析方法。以1%乙酸乙腈提取溶剂,PSA和GCB作为净化剂,超高效液相色谱分离,电喷雾电离、正离子扫描,三重四级杆串联质谱以多反应监测扫描方式进行检测,以碎片离子对m/z289.116/70.028进行定性分析、m/z 289.116/125.041进行基质匹配标准品的外标法定量。标准曲线线性方程为Y=21295x+156791,R2=0.9991,其线性范围在1~500μg·L-1。结果表明,在0.01~5mg·kg-1添加水平范围内,腈菌唑在烟草中平均回收率在88.3%~93.0%,变异系数在5.2%~7.3%,检出限(LOD)为0.029μg·kg-1,定量限(LOQ)为0.03μg·kg-1。该方法简单、快速,适用于大量烟草样品中腈菌唑的残留检测。
In this paper, Qu ECh ERS method was used to extract and purify tobacco samples. A method for the determination of myclobutanil residues in tobacco by UPLC-MS / MS was established. The solvent was extracted with 1% acetic acid in acetonitrile, and PSA and GCB were used as the purifying agent. The separation was performed by ultra performance liquid chromatography, electrospray ionization, positive ion scanning and triple quadrupole tandem mass spectrometry with multiple reaction monitoring scanning. / z289.116 / 70.028 for qualitative analysis, m / z 289.116 / 125.041 matrix matching standard external standard method. The standard curve of the linear equation Y = 21295x +156791, R2 = 0.9991, the linear range of 1 ~ 500μg · L-1. The results showed that the average recoveries of myclobutanil in tobacco ranged from 88.3% to 93.0% and the coefficients of variation ranged from 5.2% to 7.3% at the range of 0.01-5 mg · kg-1. The limit of detection (LOD) was 0.029 μg · Kg -1, and the limit of quantification (LOQ) was 0.03 μg · kg -1. The method is simple and rapid and is suitable for the determination of myclobutanil residues in a large number of tobacco samples.