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首页> 外文期刊>Chromatographia >Comparison of LC and UPLC coupled to MS-MS for the determination of sulfonamides in egg and honey
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Comparison of LC and UPLC coupled to MS-MS for the determination of sulfonamides in egg and honey

机译:LC和UPLC结合MS-MS测定鸡蛋和蜂蜜中磺胺类药物的比较

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摘要

Determination of ten sulfonamides (SAs) in egg and honey has been compared using column liquid chromatography (LC) and ultra-performance liquid chromatography (UPLC) coupled to tandem mass spectrometry (MS-MS). A liquid-liquid extraction with acetonitrile followed by solid-phase extraction on a Strata-X cartridge was developed for sample preparation. The analytical performance of both methods was compared applying the alternative matrix-comprehensive in-house validation approach using specially designed software InterVal (TM). Using UPLC the separation time was shortened about 30% reducing the run time by 8 min and a better resolution was achieved compared to LC. Due to higher peak efficiency achieved with UPLC, the decision limit values obtained by both techniques were almost equal (6.61-9.43 mu g kg(-1) and 7.25-11.9 mu g kg(-1) for UPLC and LC, respectively), despite the fact that in UPLC twice lower sample volumes were injected. Satisfactory and comparable recoveries (80-110%) were obtained by UPLC and LC for all the SAs, except for sulfacetamide by LC and sulfabenzamide by both methods. For a majority of the spiked compounds, UPLC gave significantly better precision.
机译:使用柱液相色谱(LC)和超高效液相色谱(UPLC)结合串联质谱(MS-MS)对鸡蛋和蜂蜜中十种磺酰胺(SAs)的测定进行了比较。开发了用乙腈进行液-液萃取,然后在Strata-X柱上进行固相萃取以制备样品的方法。使用专门设计的软件InterVal(TM),采用替代的矩阵综合内部验证方法,比较了这两种方法的分析性能。使用UPLC,分离时间缩短了约30%,将运行时间缩短了8分钟,与LC相比,获得了更好的分离度。由于使用UPLC可获得更高的峰效率,因此通过两种技术获得的决策极限值几乎相等(UPLC和LC分别为6.61-9.43μg kg(-1)和7.25-11.9μg kg(-1)),尽管在UPLC中进样量降低了两倍。通过UPLC和LC获得的所有SA的回收率均令人满意且可比较(80-110%),但LC和磺胺苯甲酰胺的两种方法均除外。对于大多数加标化合物,UPLC的精密度明显提高。

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