超高压液相色谱-四级杆飞行时间质谱法筛查牛奶中55种药物

Screening method for 55 kinds of drugs in milk by ultra performance liquid chromatography- quadrupole time-of-flight mass spectrometry

关键词:  牛奶  药物  筛查  超高压液相色谱-四级杆飞行时间质谱(UPLC-QTOF)

Key words:  milk  screening  drugs  UPLC-QTOF

摘要:

应用超高压液相色谱-四级杆飞行时间质谱法(UPLC-QTOF)建立了筛查牛奶中55种药物的方法。以乙腈提取样品中的药物,提取液经过HLB固相萃取柱净化浓缩后检测。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9.9×10-6。55种药物的检出限为2～10μg/kg,在5～200ng/mL范围内线性关系良好,相关系数r≥0.98。在牛奶中添加20～100μg/kg,回收率在22.9%～114.3%之间。方法操作简单,高效,杂质干扰少,适用于牛奶中55种药物的检测需要。

Abstract:

A method based on ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF) has been developed for quantitative analysis of 55 kinds of Drugs in milk. The analyte was extracted with acetonitrile, and cleaned by HLB solid phase extraction cartridge. The accurate mass was obtained in different spiking levels and the accuracy error was lower than 9.9×10-6.The limits of detection were 2 to 10μg/kg. The linearity of response ranged from 5 to 200ng/mL and the correlation coefficient was greater than 0.98. The average recoveries ranged from 22.9% to 114.3% of the fortified 55 kinds of drugs in milk at 20～100μg/kg levels. The results indicated that the method developed is easier, faster, and more sensitive. It also demonstrated that this method can meet the requirements for simultaneous determination of 55 kinds of drugs in milk.