离子色谱-质谱联用同时测定海产加工品中亚氯酸盐、氯酸盐、高氯酸盐和溴酸盐

Simultaneous determination of chlorite, chlorate, perchlorate and bromate of seafood processed products by IC-MS

建立了离子色谱-质谱联用技术同时测定海产加工品中亚氯酸盐、氯酸盐、高氯酸盐和溴酸盐的分析方法。选用高容量、亲水性的Ion Pac AS16(250 mm×2 mm)阴离子交换柱为分析柱,以EGC(自动淋洗液发生器)在线产生KOH为淋洗液,采用外接水模式,串联质谱进行检测。质谱以MRM(多元反应监测)模式分别监控以下离子对:亚氯酸盐m/z 66.9/50.8、氯酸盐m/z 84.3/68.9、高氯酸盐m/z 98.9/82.9和溴酸盐m/z 126.8/112.9,并以峰面积定量。结果表明,在一定的质量浓度范围内,4种阴离子的色谱峰面积与质量浓度呈线性相关,线性相关系数(r)均大于0.999,在1、5、10μg/L 3个加标水平下,4种目标离子的平均回收率均在89.6%~96.4%范围内,RSD(相对标准偏差)均在3.7%~5.3%之间(n=6)。该方法对亚氯酸盐、氯酸盐、高氯酸盐、溴酸盐的检出限(S/N=3)分别为0.2、0.5、0.01、0.02μg/L。上述研究表明,此方法可用于海产加工品中痕量亚氯酸盐,氯酸盐、高氯酸盐和溴酸盐的同时测定。

A method has been established for simultaneous determination of chlorite chlorate, perchlorate and bromate in seafood processed products by using ion-chromatography-electrospray tandem mass spectrometry（IC-ESI-MS） in a negative ESI mode. Chlorite, chlorate, perchlorate and bromated were separated on a high-capacity, hydrophile Ion Pac AS16（250 mm×2 mm） analysis column by gradient elution with KOH eluent generated from an eluent generator cartridge（EGC）. The MRM（multi-response monitoring） model of mass spectrometry used to monitor the following ions： chlorite m/z 66.9/50.8, chlorate m/z 84.3/68.9, perchlorate m/z 98.9/82.9 and bromate m/z 126.8/112.9. The peak area was used to quantify. Under the optimal conditions, the linear correlation coefficient was greater than 0.999. The recovery rates from spiked standard samples were in the range of 89.6%~96.4% with RSD in the range of 3.7%~5.3%（n=6）. The detection limits for chlorite, chlorate, perchlorate, bromate were 0.2, 0.5, 0.01, 0.02 μg/L. This method was proved to be sample and precise. It can be applied widely and suitable for simultaneous determination of chlorite, chlorate, perchlorate and bromate in seafood processed products.