摘要
建立了超高效液相色谱串联质谱法测定豆芽中福美双残留量的分析方法。样品经Na2EDTA-Mcllvaine缓冲溶液提取,Oasis HLB固相萃取小柱净化后,经C18色谱柱分离,乙腈-0.1%甲酸水溶液(20∶80,V/V)梯度洗脱,串联四级杆质谱检测器进行检测,基质曲线外标法定量。结果表明,福美双在2~100μg/L浓度范围内线性良好,相关系数为0.9980,检出限(S/N=3)为2.0μg/kg。在加标水平为2、6、20μg/kg时的平均加标回收率分别为93.3%,80.6%和81.9%,相对标准偏差(RSD,n=6)分别为3.47%、3.09%和1.80%。结果显示该方法操作简便,分析时间短,线性范围良好,准确度和精密度较高,净化效果好,可满足于豆芽中福美双的测定要求。
A rapid and efficient analytical method was developed for the determination of thiram in bean sprout by ultra performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS). The sample was extracted with Na2EDTA-Mcllvaine buffer solution. The extract was cleaned up with Oasis HLB. The separation of thiram was performed on a Waters ACQUITY UPLC BEH C18( 2. 1 mm i. d. ×100 mm,1. 7 μm),using 0. 1% formic acid aqueous solutionacetonitrile as mobile phase by gradient elution. The analyte was detected under positive-ion electrospray ionization mode and multi- reaction monitoring( MRM) mode. The method showed good linearity over the concentration range of 2 ~100 μg / L with correlation coefficient of 0. 9980. The limit of detection( S / N = 3) and the limit of quantification( S / N =10) were 2. 0 μg / kg and 6. 0 μg / kg,respectively. The mean recoveries at three spiked levels of 2,6,20 μg / kg were93. 3%,80. 6% and 81. 9%,respectively,with the corresponding RSDs( n = 6) of 3. 47%,3. 09% and 1. 80%,respectively. The established method showed a wide liner range and a high sensitivity,and could meet the requirements for the analysis of thiram in bean sprout.
出处
《广州化工》
CAS
2015年第21期128-130,共3页
GuangZhou Chemical Industry