超高效液相色谱-串联质谱法测定奶粉中 己烯雌酚及玉米赤霉烯酮

Determination of diethylstilbestrol and zearalenone in milk power by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  奶粉  己烯雌酚  玉米赤霉烯酮  超高效液相色谱-串联质谱法

英文关键词:milk power  diethylstilbestrol  zearalenone  ultral performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定奶粉中己烯雌酚(diethylstilbestrol, DES)及玉米赤霉烯酮(zearalenone, ZEN)的分析方法。方法 采用QuEChERS提取方法, 奶粉加水浸润后用乙腈提取, 加入氯化钠促使乙腈和水分层, 取乙腈层经中性氧化铝小柱净化。以乙腈和水作为流动相, 经ACQUITY UPLC?BEH C18色谱柱分离后, 利用超高效液相色谱-串联质谱法在电喷雾负离子模式下进行测定, 内标法定量。结果 DES和ZEN在5.0~100.0 μg/L范围内线性关系良好(r2＞0.995), 在5、10和50 μg/kg 3个加标浓度水平下, DES和ZEN的回收率在91.5%~97.5%和92.5%~95.7%之间, 相对标准偏差小于5%。结论 该方法灵敏度高, 定量准确, 可同时测定奶粉中的己烯雌酚及玉米赤霉烯酮。

英文摘要:

      Objective To establish a method for the determination of diethylstilbestrol (DES) and zearalenone (ZEN) in milk power by ultral performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The milk powder was infiltrated with water, extracted with acetonitrile by QuEChERS, and purified with neutral alumina column. The separation was achieved using a Waters UPLC?BEH C18 column and a binary gradient mobile phase of acetonitrile-water solution. The measurement was carried out by electrospray ionization (ESI) in negative mode under multiple reaction monitoring mode and quantified by internal standard method. Results The linear relation were good in the range of 5.0-100.0 μg/L (r2>0.995) for DES and ZEN. The recoveries of DES and ZEN were respectively in the range 91.5%-97.5% and 92.5%-95.7%, at 3 spiked concentrations of 5, 10 and 50 μg/kg. The relative standard deviations were less than 5%. Conclusion This method is sensitive and accurate, which is suitable for simultaneous determination of diethylstilbestrol and zearalenone in milk power.