液相色谱串联质谱法测定饲料中高氯酸盐含量

Determination of perchlorate in feed by liquid chromatography tandem mass spectrometry

中文关键词:  饲料  高氯酸盐  液质联用  同位素内标法  含量检测

英文关键词:forage  perchlorate  liquid chromatography-tandem mass spectrometry  isotopic internal standard method  content determination

中文摘要:

      目的 建立液相色谱串联质谱检测饲料中高氯酸盐含量的方法。方法 饲料样品经乙腈-水(2:1,V:V)超声提取, 高速离心后, 上清液经石墨炭黑固相萃取柱净化, 液相色谱串联质谱测定, 内标法定量。结果 高氯酸盐在0 ~100 ng/mL浓度范围内呈良好线性关系(r2=0.9998)。本方法的定量限为15.0 μg/kg。高氯酸盐在15~150 μg/kg添加浓度范围内, 回收率为95.1%~102.4%, 相对标准偏差为1.13%~9.82%。结论 本方法前处理简单, 具有较高准确度、灵敏度、稳定性, 可以满足饲料中高氯酸盐的含量检测。

英文摘要:

      Objective To established a method for the determination of perchlorate content in forage by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods Samples of forage were ultrasound extracted by acetonitrile - aqueous solution (2:1, V:V) and centrifugated at a high speed. Then the supernatant was purified by graphitized carbon black solid phase extraction column, and determined by LC-MS/MS, then quantified by internal standard method. Results The perchlorate showed a good linear relationship in the concentration range of 0– 100 ng/mL (r2=0.9998). The quantitative limit of the method was 15.0 μg/kg. The recoveries rate of perchlorate in the range of 15–150 μg/kg was 95.1%-102.4% and relative standard deviations were 1.13%–9.82%.Conclusion This method has the advantages of simple pretreatment, high accuracy, sensitivity and stability, and can satisfy the determination of perchlorate content in feed.