液相色谱串联质谱法测定饲料中高氯酸盐含量
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。
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.
标题：液相色谱串联质谱法测定饲料中高氯酸盐含量
英文标题：Determination of perchlorate in feed by liquid chromatography tandem mass spectrometry
作者：
马晓冲 君乐宝乳业集团农业农村部乳品质量安全控制重点实验室
王瑶 君乐宝乳业集团农业农村部乳品质量安全控制重点实验室
李兴佳 君乐宝乳业集团农业农村部乳品质量安全控制重点实验室
柴艳兵 君乐宝乳业集团农业农村部乳品质量安全控制重点实验室
张耀广 君乐宝乳业集团农业农村部乳品质量安全控制重点实验室
李飞 君乐宝乳业集团农业农村部乳品质量安全控制重点实验室
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,
发表日期：2020-03-31
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