Zhang Xiaoguang, Liu Dong, Liu Hongran, Li Qiang, Li Lili, Wang Lixia, Zhang Yan
Hebei Food Inspection and Research Institute, Key Laboratory of Food Safety of Hebei Province, Shijiazhuang 050091, China.
Shijiazhuang Food and Drug Inspection Institute, Shijiazhuang 050011, China.
Se Pu. 2017 Oct 8;35(10):1055-1061. doi: 10.3724/SP.J.1123.2017.04004.
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method based on-line solid phase extraction (SPE) purification was established to determine 10 macrolide antibiotics in pork samples. The samples were extracted with acetonitrile, and the extracts were dried with rotary evaporator at 40℃, then the analytes were dissolved with 2 mL phosphate buffer. The solutions were purified and concentrated by on-line SPE with HLB cartridges. The analytes were eluted with methanol, and then transferred to XBridge BEH C18 column, separated with the mobile phases of 10 mmol/L ammonium acetate aqueous solution and acetonitrile. Finally, the target analytes were detected by tandem mass spectrometry. The results showed that good linearity was obtained in the range of 0.1-200 μg/L for the 10 macrolide antibiotics with correlation coefficients better than 0.990. The limits of detection were in range of 0.05-0.30 μg/kg and the limits of quantitation were in range of 0.10-1.00 μg/kg. The recoveries of the method were in range of 69.6%-115.2% at the spiked levels of 0.10-10.0 μg/kg for all analytes, with the relative standard deviations less than 10%. The developed method can be used for the determination of the 10 macrolide antibiotics in pork samples.
建立了一种基于在线固相萃取（SPE）净化的高效液相色谱-串联质谱（HPLC-MS/MS）方法，用于测定猪肉样品中的10种大环内酯类抗生素。样品用乙腈提取，提取物在40℃下用旋转蒸发仪干燥，然后用2 mL磷酸盐缓冲液溶解分析物。溶液通过HLB柱在线SPE进行净化和浓缩。分析物用甲醇洗脱，然后转移至XBridge BEH C18柱，用10 mmol/L醋酸铵水溶液和乙腈作为流动相进行分离。最后，通过串联质谱检测目标分析物。结果表明，10种大环内酯类抗生素在0.1 - 200 μg/L范围内具有良好的线性，相关系数优于0.990。检测限在0.05 - 0.30 μg/kg范围内，定量限在0.10 - 1.00 μg/kg范围内。在0.10 - 10.0 μg/kg的加标水平下，该方法对所有分析物的回收率在69.6% - 115.2%范围内，相对标准偏差小于10%。所建立的方法可用于测定猪肉样品中的10种大环内酯类抗生素。
