同位素稀释超高效液相色谱-串联质谱法测定怀山药中的高氯酸盐和氯酸盐

Determination of perchlorate and chlorate in Dioscoreae Rhizoma by isotope dilution ultra high performance liquid chromatography tandem mass spectrometry

目的采用同位素稀释超高效液相色谱-串联质谱法测定怀山药中的高氯酸盐和氯酸盐的方法对焦作市怀山药中的高氯酸盐和氯酸盐的含量进行测定。方法样品用80%乙腈-水溶液提取,提取液过固相萃取柱经净化后采用Waters TorusTM DEA超高效色谱柱(150 mm×2.1 mm,1.7μm),流动相为乙腈-0.1%甲酸水溶液进行梯度洗脱,柱温30℃,流速0.3 ml/min,以非诺特罗作为内标进行定量。结果高氯酸盐和氯酸盐分别在1~100μg/L和2~200μg/L的浓度范围内线性良好,相关系数r>0.9997。高氯酸盐和氯酸盐的检出限分别为1μg/kg和2μg/kg;样品加样回收率分别为99.8%和99.4%,相对标准偏差为2.3%和2.8%。结论本方法简便、快捷、灵敏、准确,能够满足怀山药中的高氯酸盐和氯酸盐含量测定要求。

Objective To estabilish an isotope dilution ultra-high performance liquid chromatography tandem mass spectrometry method for the determination of perchlorate and chlorate in Dioscoreae Rhizoma and to deter-mine the contents of perchlorate and chlorate in Huai rhizoma in our city.Methods Samples were extract-ed with 80%acetonitrile-water solution.The extracts were purified by SPE,seperated by UPLC on the Water TorusTM DEA column(150 mm×2.1 mm,1.7μm),with the mobile phase of acetonitrile-0.1%formic acid aque-ous solution in a gradient elution,at a column temperature of 30°C,and the flow rate of 0.3 ml/min,and quanti-fied by the use of Fenoterol as an internal standard.Results Chlorate and perchlorate showed a good linearity(r>0.999)in the range of 1-100μg/L and 2-200μg/L,respectively.The LOD for chlorate and perchlorate were 1.0μg/kg and 2μg/kg.The relative standard deviations were 2.3%and 2.8%.Conclusion This method is sim-ple,Quick,sensitive and accurate.It is suitable for determination of perchlorate and chlorate in Dioscorea Rhi-zoma.