Determination of Zearalenone and Its Metabolites in Milk Powder by HPLC-MS/MS with QuEChERS Cleanup
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摘要: 建立了QuEChERS-高效液相色谱-串联质谱同时检测奶粉中玉米赤霉烯酮及其代谢产物的检测方法。样品用10 mL超纯水溶解,1%乙酸乙腈溶液提取,乙酸钠盐析,C18、N-丙基乙二胺(primary secondary amine,PSA)和无水硫酸镁净化,在ZORBAX SB-C18色谱柱上分离,以5 mmol/L乙酸铵溶液和乙腈作为流动相进行梯度洗脱,ESI负离子模式扫描,多反应监测(MRM)测定,β-玉米赤霉烯醇内标法定量分析。奶粉中玉米赤霉烯酮及其代谢产物在0.1~50 μg/L浓度范围内呈线性关系,相关系数均高于0.999,基质效应为抑制效应;检出限(LOD)均为0.1 μg/kg,定量限(LOQ)均为0.2 μg/kg。奶粉中玉米赤霉烯酮及其代谢产物的3个加标浓度水平的平均回收率范围为85.2%~119.3%,相对标准偏差(RSD)在0.3%~12.2%(n=7)之间。该方法简便快速、准确可靠,可用于检测奶粉中玉米赤霉烯酮及其代谢物。
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关键词:
- 奶粉 /
- 玉米赤霉烯酮 /
- QuEChERS /
- 高效液相色谱-串联质谱
Abstract: A method for simultaneous determination of zearalenone and its metabolites(ZERs)in milk powder was developed by high performance liquid chromatography-tandem mass spectrometry with QuEChERS cleanup. The sample was diluted with 10 mL ultra-pure water,extracted by 1% acetonitrile acetate,and sodium acetate salting out,cleaned up with C18,PSA and mgnesium sulfate anhydrous. The analytes were separated by a reversed phase C18 column and gradiently eluted with 5 mmol/L ammonium acetate and acetonitrile. The determination was conducted by negative electrospray ionization(ESI-)with the multiple reaction monitoring(MRM)mode. The ZERs was quantified by internal standard method with β-zearalenol-d7. The good linearities were obtained for ZERs at the concentration of 0.1~50 μg/L with the linear correlation coefficients more than 0.999,and the matrix effect was inhibition. The limits of detection(LOD)and the limits of quantification(LOQ)for ZERs were 0.1 μg/kg and 0.2 μg/kg,respectively. The recoveries at three concentration spiked levels were in the range of 85.2%~119.3%. The repeatability expressed as relative standard deviations(RSD)was ranged from 0.3% to 12.2%(n=7). The method is simple,rapid,accurate and reliable,and can be used for detecting ZERs in milk powder.
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