摘要
建立了高效液相色谱-串联质谱法同时测定肉类中氯酸盐和高氯酸盐的分析方法。样品经乙腈-水(13:7,V:V)提取后离心,上清液经PRiME HLB固相萃取柱净化,Acclaim Trinity P1复合离子交换柱分离,以乙腈及20 mmol/L乙酸铵为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式,内标法定量。结果表明,氯酸盐和高氯酸盐分别在2~200.0 ng/mL、1~100.0 ng/mL范围内呈现良好线性关系,决定系数分别为0.9983和0.9998,方法的定量限分别为2.0、1.0μg/kg。氯酸盐和高氯酸盐分别在三种肉类四个添加水平6.0、20、40、200μg/kg和3.0、10、20、100μg/kg的加标回收率为91.0%~105.7%和94.2%~110.5%,相对标准偏差为1.8%~9.7%和0.7%~9.4%。本方法具有操作简单、灵敏度高、稳定性好等优点,可很好地满足肉中氯酸盐、高氯酸盐的检测。
A method for simultaneous determination of chlorate and perchlorate amounts in meat by high performance liquid chromatography-tandem mass spectrometry was developed.Samples were extracted with acetonitrile/water(13:7,V:V)and centrifuged.The obtained supernatants were purified on a PRiME HLB solid phase extraction column,followed by an Acclaim Trinity P1 ion exchange column with the gradient elution of acetonitrile and 20 mmol/L ammonium acetate as the mobile phase to afford chlorate and perchlorate.MS/MS was performed in ESI+and multiple reaction monitoring mode with an internal standard for quantification.The results showed chlorate and perchlorate had calibration curves with good linearity in the ranges of 2~200.0 ng/mL and 1~100.0 ng/mL respectively,with corresponding correlation coefficients being 0.9983 and 0.9998.The detection limits of the method were 2.0 and 1.0μg/kg,respectively.The recovery rates of chlorate and perchlorate were 91.0%~105.7%and 94.2%~110.5%respectively,at the addition levels of 6.0,20,40,200μg/kg,and 3.0,10,20,100μg/kg.The relative standard deviations for chlorate and perchlorate were 1.8%~9.7%and 0.7%~9.4%respectively.This method would be easy to use and has high detection sensitivity and good stability,and could well meet the requirements of determining chlorate and perchlorate amounts in meat.
作者
于艳丽
李杰
YU Yanli;LI Jie(Shanghai Sanda University,Shanghai 201209,China;Shanghai Denuo Product Service Co.,Ltd.,Shanghai 200436,China)
出处
《食品工业科技》
CAS
北大核心
2023年第11期265-270,共6页
Science and Technology of Food Industry
基金
上海杉达学院科研基金项目(2022YB05)。
关键词
氯酸盐
高氯酸盐
高效液相色谱-串联质谱法
肉类
chlorate
perchlorate
high performance liquid chromatography-tandem mass spectrometry
meat