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

作　　者：王珍妮 陈颖[1] 宋月[1] 白欣[1] WANG Zhen-ni;CHEN Ying;SONG Yue;BAI Xin(Department of Physical and Chemical Testing,Dalian Center for Disease Control and Prevention,Dalian,Liaoning 116021,China)

机构地区：[1]大连市疾病预防控制中心理化技术检验科,辽宁大连116021

出　　处：《中国卫生工程学》2024年第4期455-457,共3页Chinese Journal of Public Health Engineering

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,PRiMEHLB固相萃取柱净化,以WatersTorusDEA色谱柱(2.1mm×100mm,1.7μm)为分离柱,乙腈和20mmol/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2~200ng/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1.0μg/kg和0.5μg/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。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 mmx100 mm,1.7μm).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 1.0μg/kg for chlorate and 0.5μg/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 

分 类 号：R155[医药卫生—营养与食品卫生学] O657.63[医药卫生—公共卫生与预防医学]