陈秀梅，闫慧娟，张晓敏，蔺婷娟，胡雪，孟根花*
（内蒙古伊利实业集团股份有限公司，内蒙古呼和浩特 010110）
摘要：建立了乳与乳制品中氯酸盐和高氯酸盐的超高效液相色谱-串联质谱联用的检测方法。试样中的目标物经0.1%甲酸水提取，乙腈沉淀蛋白，PRIME HLB 固相萃取柱净化，Amide 色谱柱分离，以10mmol 乙酸铵溶液和乙腈为流动相进行梯度洗脱，在电喷雾电离源负离子（ESI-）多反应监测模式下，采用同位素内标法进行定性和定量分析。结果表明：高氯酸盐和氯酸盐分别在0.5μg/L～50μg/L 和5μg/L～500μg/L 范围内线性关系良好，高氯酸盐和氯酸盐的定量限分别为7.5μg/kg 和15μg/kg。在7.5、15、30μg/kg 三种加标水平下，高氯酸盐在乳与乳制品中的平均回收率为88.1%～107.6%，相对标准偏差2.2%～4.1%。在15、30、150μg/kg 三种加标水平下，氯酸盐在乳与乳制品中的平均回收率为80.1%～102.8%，相对标准偏差2.4%～3.7%。该法操作简单，检测速度快、结果稳定可靠，适用于乳与乳制品中氯酸盐和高氯酸盐的检测。
关键词：氯酸盐；高氯酸盐；乳与乳制品；超高效液相色谱-串联质谱法
Determination of Chlorate and Perchlorate Residues in Milk and Dairy Products by UltraPerformance Liquid Chromatography-Tandem Mass Spectrometry
CHEN Xiu-mei，YAN Hui-juan，ZHANG Xiao-min，LIN Ting-juan，HU Xue，MENG Gen-hua*
（Inner Mongolia Yili Industrial Group Limited by Share Ltd，Huhhot 010110，China）
Abstract: A method for the determination of chlorate and perchlorate in milk and dairy products by ultra performanceliquid chromatography-mass spectrometry mass spectromtery（UPLC-MS/MS）was established. The target compoundswere extracted with 0.1% formic acid water，precipitated by acetonitrile，purified by PRIME HLB solid phaseextraction column，and separated by an Amide column. Gradient elution was performed with 10mmol ammoniumacetate solution and acetonitrile as the mobile phase. Qualitative and quantitative analysis was carried out by isotopeinternal standard method in ESI- multi- reaction monitoring mode. The results showed that the linear range ofperchlorate and chlorate was 0.5μg/L～50μg/L and 5μg/L～500μg/L，respectively. The limits of quantification ofperchlorate and chlorate were 7.5μg/kg and 15μg/kg，respectively. At the spiked levels of 7.5，15 and 30g/kg，Theaverage recoveries of perchlorate in milk and dairy products ranged from 88.1% to 107.6% with relative standarddeviations（RSD%）of 2.2% to 4.1%. At the spiked levels of 15，30 and 150μg/kg，the average recoveries of chloratein milk and dairy products were 80.1% to 102.8% with relative standard deviations（RSD%）of 2.4% to 3.7%. Themethod is simple，fast，stable and reliable. It is suitable for the determination of chlorate and perchlorate in milk anddairy products.
Key words: chlorate；perchlorate；milk and dairy products；ultra performance liquid chromatography-mass spectrometrymass spectrometry（UPLC-MS/MS）
中图分类号：TS252.7 文献标志码：A 文章编号：1007-7871（2023）03-0019-06
2023，Vol.26，No.3