液相色谱-串联质谱法同时测定鸡肉中的螺旋霉素(I型)和新螺旋霉素

Simultaneous determination of spiramycin(I) and neospiramycin in chicken by liquid chromatography-tandem mass spectrometry

中文关键词:  螺旋霉素(I型)  新螺旋霉素  鸡肉  液相色谱-串联质谱法

英文关键词:spiramycin(I)  neospiramycin  chicken  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立鸡肉中螺旋霉素(I型)和新螺旋霉素的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测方法。方法 样品经磷酸盐缓冲溶液(0.1 mol/L, pH=8.0)提取, 正己烷脱脂后, 经HLB固相萃取柱净化, 氮吹浓缩, 采用LC-MS/MS, 在正离子模式下进行检测。结果 该方法在螺旋霉素(I型)和新螺旋霉素的浓度为0~200 μg/kg范围内有良好的线性关系, 相关系数r>0.995, 定量限均为10 μg/kg。螺旋霉素(I型)和新螺旋霉素在3个不同添加水平下的平均回收率为87.1%~102%, 相对标准偏差为3.45%~6.56%。结论 该方法简便、快速, 准确度和精密度良好, 可以满足鸡肉中螺旋霉素(I型)和新螺旋霉素的测定需要。

英文摘要:

      Objective To establish a method for the determination of spiramycin(I) and neospiramycin in chicken by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were extracted with phosphate buffer solution (0.1 mol/L, pH=8.0), and the fat in samples were removed by n-hexane. The obtained extract was purified by HLB solid phase extraction column, concentrated by nitrogen blowing instrument, and then detected by LC-MS/MS with positive ion mode. Results The method showed good linearities when the concentration of spiramycin(I) and neospiramycin ranged from 0~200 μg/kg, the correlation coefficients were both greater than 0.995, and the limits of quantitation were both 10 μg/kg. The average recoveries of spiramycin(I) and neospiramycin at 3 spiked levels were 87.1%~102%, and the relative standard deviations were 3.45%~6.56%. Conclusion This method is simple and rapid with good accuracy and precision, which is suitable for the detection of spiramycin(I) and neospiramycin in chicken.