Xia Xi, Li Xiaowei, Ding Shuangyang, Zhang Suxia, Jiang Haiyang, Li Jiancheng, Shen Jianzhong
Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing, China.
J Chromatogr A. 2009 Mar 20;1216(12):2587-91. doi: 10.1016/j.chroma.2009.01.033. Epub 2009 Jan 17.
This work reports a rapid, reliable and sensitive multi-residue method for the simultaneous determination of six resorcylic acid lactones in bovine milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The resorcylic acid lactones were extracted, purified, and concentrated from milk samples in one step using a solid-phase extraction (SPE) cartridge that contained a polymeric mixed-mode anion-exchange sorbent. The analysis was performed on a Waters Acquity BEH C(18) column utilizing a gradient elution profile. Each LC run was completed in 3.5 min. The analytes were detected by multiple reaction monitoring (MRM) using electrospray ionization (ESI) negative mode. Mean recoveries from fortified samples ranged from 92.6% to 112.5%, with relative standard deviations lower than 11.4%. Using 5 mL bovine milk, the limits of detection and quantification for resorcylic acid lactones were in the ranges of 0.01-0.05 and 0.05-0.2 microg/L, respectively. The application of this newly developed method was demonstrated by analyzing bovine milk samples from markets.
本研究报道了一种快速、可靠且灵敏的多残留方法，用于通过超高效液相色谱-串联质谱法（UHPLC-MS/MS）同时测定牛奶中的六种间苯二酚内酯。使用含有聚合物混合模式阴离子交换吸附剂的固相萃取（SPE）柱，一步从牛奶样品中提取、纯化并浓缩间苯二酚内酯。分析在Waters Acquity BEH C(18)柱上进行，采用梯度洗脱模式。每次液相色谱运行在3.5分钟内完成。通过电喷雾电离（ESI）负离子模式下的多反应监测（MRM）检测分析物。加标样品的平均回收率在92.6%至112.5%之间，相对标准偏差低于11.4%。使用5 mL牛奶，间苯二酚内酯的检测限和定量限分别在0.01-0.05和0.05-0.2 μg/L范围内。通过分析市售牛奶样品证明了该新开发方法的应用。
