高效液相色谱-串联质谱法测定黄喉中五氯酚酸钠的含量

Determination of pentachlorophenol sodium in Huanghou by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  五氯酚酸钠  黄喉  高效液相色谱-串联质谱法  外标法

英文关键词:pentachlorophenol sodium  Huanghou  high performance liquid chromatography-tandem mass spectrometry  external standard method

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)测定黄喉中五氯酚酸钠含量的方法。方法 样品通过8 mL 8%的三乙胺乙腈水溶液(8:2, V:V)涡旋振荡重复提取2次, 上清液经Bond Elut Plexa PAX柱净化, 以0.05%甲酸水+乙腈为流动相梯度洗脱, 多反应监测负离子模式扫描, 外标法定量。结果 五氯酚酸钠在1~100 ng/mL范围内线性关系良好, 相关系数大于0.995, 检出限为0.25 μg/kg, 定量限为0.5 μg/kg, 不同添加水平的平均回收率为90.4%~95.7%, 相对标准偏差小于5%。结论 该方法可以达到快速、准确、稳定的分析效果, 适用于黄喉中五氯酚酸钠的测定。

英文摘要:

      Objective To establish a method for determination of pentachlorophenol sodium in Huanghou by high performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS). Methods The sample was extracted twice with 8 mL 8% triethylamine acetonitrile aqueous solution (8:2, V:V) by vortex oscillation. The supernatant was purified by the Bond Elut Plexa PAX column using 0.05% formate water+acetonitrile as the mobile phase for gradient elution. The sample was detected under the multiple reaction monitoring mode with negative electrospray ionization, and quantified by the external standard methods. Results Pentachlorophenol sodium had a good linear relationship in the range of 1?100 ng/mL, and the correlation coefficient was greater than 0.995. The limit of detection was 0.25 μg/kg, and the limit of quantitation was 0.5 μg/kg. The average recovery rates of different addition levels were 90.4%?95.7%, and the relative standard deviation was less than 5%. Conclusion This method can achieve fast, accurate and stable analysis effect and is suitable for the determination of pentachlorophenol sodium in Huanghou.