Tölgyesi Adám, Fekete Jenõ, Fekete Szabolcs, Sharma Virender K, Békési Katalin, Tóth Edina
Central Agricultural Office Food and Feed Safety Directorate, Food Toxicology National Reference Laboratory, Budapest, Hungary.
J Chromatogr Sci. 2012 Mar;50(3):190-8. doi: 10.1093/chromsci/bmr046.
A fast liquid chromatography-tandem mass spectrometry (LC-MS-MS) method is developed to determine lincomycin (LM) in honey, muscle, milk, and egg. Samples are cleaned-up at pH 4.7 using Strata-X-C mixed-mode polymeric strong cation exchange solid-phase extraction (SPE) cartridges, which could selectively adsorb the lincomycin from matrices under the acidic condition. LM is separated on the recently introduced Kinetex XB core-shell type HPLC column using isocratic elution mode with a mobile phase containing 0.1% formic acid in water/acetonitrile (93/7, v/v, pH 2.6) at a flow rate of 0.7 mL/min. The subsequent MS/MS detection has decreased ion effect, which allows the limit of detection (LOD) of LM for honey to be 0.05 µg/kg for honey and 0.5 µg/kg for muscle, milk, and egg. These LODs are much lower than those reported previously. The other main advantage of the developed method is the analysis time of only 3.5 min, which is about three times shorter than other reported LC-MS-MS methods. Recoveries varies between 94.2% and 125.2% and in-house reproducibility ranges from 3.7% to 28.7%. The developed method is validated according to European Union (EU) Commission Decision 2002/657/EC using a matrix-comprehensive validation strategy. All studied analytical parameters fulfills the EU guidelines.
建立了一种快速液相色谱-串联质谱（LC-MS-MS）方法，用于测定蜂蜜、肌肉、牛奶和鸡蛋中的林可霉素（LM）。使用Strata-X-C混合型聚合强阳离子交换固相萃取（SPE）小柱在pH 4.7条件下对样品进行净化处理，该小柱能够在酸性条件下从基质中选择性吸附林可霉素。采用等度洗脱模式，在最近推出的Kinetex XB核壳型高效液相色谱柱上分离LM，流动相为含0.1%甲酸的水/乙腈（93/7，v/v，pH 2.6），流速为0.7 mL/min。随后的MS/MS检测降低了离子效应，使得蜂蜜中LM的检测限（LOD）为0.05 µg/kg，肌肉、牛奶和鸡蛋中为0.5 µg/kg。这些检测限远低于先前报道的值。所开发方法的另一个主要优点是分析时间仅为3.5分钟，比其他报道的LC-MS-MS方法短约三倍。回收率在94.2%至125.2%之间，内部重现性范围为3.7%至28.7%。所开发的方法根据欧盟委员会第2002/657/EC号决定，采用基质全面验证策略进行了验证。所有研究的分析参数均符合欧盟指南。
