高效液相色谱-串联质谱法测定液体乳中氯酸盐和高氯酸盐

Determination of chlorate and perchlorate in liquid milk by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  复合阴离子交换柱  氯酸盐  高氯酸盐  液体乳  高效液相色谱-串联质谱法

英文关键词:composite anion exchange column  chlorate  perchlorate  liquid milk  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定液体乳中的氯酸盐和高氯酸盐的分析方法。方法 样品经0.2%甲酸水-甲醇(10:90, V:V)提取, HLB固相萃取柱净化。经Acclaim Trinity P1复合阴离子交换柱(100 mm×2.1 mm, 3 μm)洗脱。在流速0.5 mL/min下以乙腈-20 mmoL/L甲酸铵溶液(70:30, V:V)作为流动相, 梯度分离。采用三重四极杆电喷雾离子源电离-多反应监测(multiple reaction monitoring, MRM)-负离子监测模式检测, 分别以氯酸根-18O3高氯酸根-18O4为内标物, 进行内标法定量。结果 氯酸盐和高氯酸盐分别在0.0~50.0 μg/kg和0.0~25.0 μg/kg范围内线性关系良好, 相关系数r2都大于0.999。方法的测定低限分别为0.4 μg/kg和0.6 μg/kg。回收率为80.0%~93.6%, 相对标准偏差(relative standard deviation, RSD)为2.14%~6.68%, 结论 该方法提取率高, 准确可靠, 适用于液体乳中氯酸盐和高氯酸盐的定量分析。

英文摘要:

      Objective To establish a method for the determination of chlorate and perchlorate in liquid emulsion by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted by 0.2% formate water and methanol (10:90, V:V) and purified by HLB solid phase extraction column. The Acclaim Trinity P1 composite anion exchange column (100 mm×2.1 mm, 3 μm) was used for elution. Acetonitrile-20 mmol/L ammonium formate (70:30, V:V) was used as the mobile phase at the flow rate of 0.5 mL/min for gradient separation. Triple quadrupole electrospray ion source (ESI source) ionization-multiple reaction monitoring (MRM)-anion monitoring mode was used for detection. Using -18O3 and -18O4 as internal standards, internal standard method was used for quantitative analysis. Results The linear relationships of chlorate and perchlorate were good in the ranges of 0.0?50.0 g/kg and 0.0?25.0 g/kg, respectively, and the correlation coefficients r2 were greater than 0.999. The lower limits of the method were 0.4 μg/kg and 0.6 μg/kg, respectively. The recovery rates were 80.0%?93.6%, and relative standard deviations (RSDs) were 2.14%?6.68%. Conclusion The experimental results showed that the method had a high extraction rate, was accurate and reliable, and was suitable for the quantitative analysis of chlorate and perchlorate in liquid milk.