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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。
The analytical method of simultaneous determination of chlorite, chlorate, perchlorate and bromate in seafood products by ion chromatography-mass spectrometry was established. A high capacity, hydrophilic Ion Pac AS16 (250 mm × 2 mm) anion exchange column was used as the analytical column. KOH was generated on-line with EGC (Automatic Eluent Generator). The external water mode and tandem mass spectrometry Test. Mass spectra The following ion pairs were monitored in MRM (multiple reaction monitoring) mode: 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, and was quantified as peak area. The results showed that the chromatographic peak areas of the four anions were linearly correlated with the mass concentrations within a certain range of mass concentration. The linear correlation coefficients (r) were all greater than 0.999. Under the three spiked levels of 1, 5, and 10 μg / L, The average recoveries of the four target ions ranged from 89.6% to 96.4% with RSDs of 3.7% -5.3% (n = 6). The detection limits (S / N = 3) for chlorite, chlorate, perchlorate and bromate were 0.2, 0.5, 0.01 and 0.02 μg / L respectively. The above study shows that this method can be used for the simultaneous determination of trace amounts of chlorite, chlorate, perchlorate and bromate in seafood products.