超高效液相色谱-三重四级杆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 ultra performance liquid chromatography-triple quadrupole mass spectrometry
王珍妮 1陈颖 1宋月 1白欣1
作者信息
- 1. 大连市疾病预防控制中心理化技术检验科,辽宁 大连 116021
- 折叠
摘要
目的 建立超高效液相色谱-三重四级杆串联质谱法快速测定液体乳中氯酸盐和高氯酸盐的方法.方法 样品经乙腈提取,PRiME HLB固相萃取柱净化,以Waters Torus DEA色谱柱(2.1 mmx100 mm,1.7 μm)为分离柱,乙腈和20 mmol/L乙酸铵溶液为流动相梯度洗脱,采用超高效液相色谱-串联四极杆质谱仪测定,内标法定量.结果 氯酸盐和高氯酸盐分别在2～200 ng/ml和1～100ng/ml内呈现良好线性,相关系数均＞0.99,检出限分别为1.0 μg/kg和0.5 μg/kg,平均回收率分别为91.0％～95.6％和92.5％～95.4％,相对标准偏差分别为4.55％～5.70％(n=6)和4.34％～5.81％(n=6).结论 该方法操作简单,灵敏度高,重现性好,适用于液体乳中氯酸盐和高氯酸盐的测定,为食品安全国家标准的建立提供准确有效的数据支持.
Abstract
Objective To establish an ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-TQMS)method for rapid determination of chlorate and perchlorate in liquid milk.Methods The samples were ex-tracted with acetonitrile,purified by PRiME HLB solid-phase extraction column and separated with a Waters Torus DEA column(2.1 mm×100 mm,1.7 μm).Acetonitrile and 20 mmol/L ammonium acetate solution were used as mobile phases for gradient elution.The analytes were detected by UPLC-TQMS and quantified by the internal standard method.Results The calibration curves showed a good linear relationship in the range of 2-200 ng/ml for chlorate and 1-100 ng/ml for per-chlorate with the correlation coefficient greater than 0.99.The limit of detection was 1.0 μg/kg for chlorate and 0.5 μg/kg for perchlorate.The average recoveries of chlorate and perchlorate were 91.0％ -95.6％ and 92.5％ -95.4％ ,respectively.The relative standard deviations of chlorate and perchlorate were 4.55％ -5.70％ (n=6)and 4.34％ -5.81％ (n=6),re-spectively.Conclusion The method is simple and sensitive with high reproducibility,which is suitable for the determination of chlorate and perchlorate in liquid milk.Furthermore,it provides an accurate and effective data support for the establishment of the national food safety standards.
关键词
液体乳/氯酸盐/高氯酸盐/固相萃取/超高效液相色谱-三重四级杆串联质谱法Key words
Liquid milk/Chlorate/Perchlorate/Solid-phase extraction/Ultra performance liquid chromatography-triple quadrupole mass spectrometry引用本文复制引用
出版年
2024
NETL
NSTL
万方数据