高效液相色谱-四极杆-飞行时间质谱测定婴幼儿配方奶粉中的高氯酸盐
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摘要
建立了高效液相色谱-四极杆-飞行时间质谱法(HPLC-Q-TOF/MS)测定婴幼儿配方奶粉中高氯酸盐的分析方法。优化了色谱质谱条件以及样品提取和净化条件。在优化条件下,以高分辨多反应监测(MRM HR)模式扫描,同位素内标法定量,实现了婴幼儿配方奶粉中高氯酸盐的精确定量分析。高氯酸盐在0. 5～50 ng/mL范围内线性关系良好,相关系数为0. 9999。方法检出限为0. 75μg/kg,定量限为2. 5μg/kg,在3个添加水平下的回收率为95. 4%～101. 9%,相对标准偏差(RSD)为2. 4%～7. 5%(n=6)。该方法适用于婴幼儿配方奶粉中高氯酸盐的测定。
An analytical method for accurate quantification of perchlorate in infant formulas was developed by high-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry( HPLC-Q-TOF/MS). The HPLC-Q-TOF/MS conditions and sample preparation procedure were optimized. Under the optimal conditions,multiple reaction monitoring high-resolution( MRM HR) acquisition was performed to accurately quantify perchlorate in infant formulas with isotope-labelled internal standard method. The results exhibited a good linearity in the range of 0. 5-50 ng/m L,with the correlation coefficients( r) of 0. 9999. The limits of detection( LODs,S/N = 3)was 0. 75 μg/kg,and the limits of quantitation( LOQs,S/N = 10) was 2. 5 μg/kg. The recoveries of perchlorate at three spiked levels varied from 95. 4% to 101. 9% with the relative standard deviations( RSDs) ranging from 2. 4% to 7. 5%( n = 6). The method is suitable for the rapid determination of perchlorate in infant formulas.
An analytical method for accurate quantification of perchlorate in infant formulas was developed by high-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry( HPLC-Q-TOF/MS). The HPLC-Q-TOF/MS conditions and sample preparation procedure were optimized. Under the optimal conditions,multiple reaction monitoring high-resolution( MRM HR) acquisition was performed to accurately quantify perchlorate in infant formulas with isotope-labelled internal standard method. The results exhibited a good linearity in the range of 0. 5-50 ng/m L,with the correlation coefficients( r) of 0. 9999. The limits of detection( LODs,S/N = 3)was 0. 75 μg/kg,and the limits of quantitation( LOQs,S/N = 10) was 2. 5 μg/kg. The recoveries of perchlorate at three spiked levels varied from 95. 4% to 101. 9% with the relative standard deviations( RSDs) ranging from 2. 4% to 7. 5%( n = 6). The method is suitable for the rapid determination of perchlorate in infant formulas.
引文
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