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超高压液相色谱串联四级杆飞行时间质谱法同时筛查牛肉中6种镇静剂
吴宁鹏
0
(河南省兽药监察所)
摘要:
应用超高压液相色谱串联四级杆飞行时间质谱建立了测定牛肉中6种镇静剂的新方法。样品通过乙腈两次提取,旋蒸后通过氨基柱除脂净化。在不同添加浓度下获得了精确分子离子质量,质量偏差的绝对值低于7?10-6。6种镇静剂的检出限为0.5μg/kg~1μg/kg,在不同浓度下测定了6种镇静剂的回收率,回收率在60%~90%之间,6种药物在2ng/ml~50ng/ml范围内线性关系良好,相关系数r2≥0.98。该方法适用于牛肉中6种镇静剂的检测需要,该方法操作简单,准确,杂质干扰少。
关键词:  镇静剂  筛查  牛肉  超高效液相色谱-飞行时间质谱
DOI:
投稿时间:2013-05-03修订日期:2013-06-25
基金项目:
Sreening of 6 sedatives in beef by ultra performance liquid chromatography- quadrupole time-of-flight mass spectrometry
(Henan Institμte of Veterinary Drμg Control)
Abstract:
A method for scrreening of 6 sedatives in beef by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF) has been developed. The sedatives were extracted by acetonoitrile for twice and purified by NH2 cartridge. The accurate mass was obtained under different levels and the accuracy error was lower than 7?10-6. The correlations of 6 sedatives were greater than 0.98 between 2ng/ml and 50ng/ml. The limits of detection of 6 sedatives were from 0.5μg/kg to 1μg/kg. The average recoveries ranged from 60% to 90% of the fortified 6 sedatives in beef at 2~10μg/kg levels. The results showed that the method was highly sensitive and selective for screening of 6 sedatives in beef.
Key words:  sedatives  screening  beef  ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF)

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