摘要
目的选择固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中链霉素残留最佳测定条件。方法样品用EDTA-Na2缓冲溶液提取,应用强阳离子交换固相萃取柱(MCX)前处理净化技术,通过对样品中待测组分的提取、净化后,采用HILIC色谱柱(50 mm×2.1 mm,1.7μm)分离,以乙腈和含0.1%甲酸的20 mmol/L乙酸铵溶液梯度洗脱,正离子电喷雾离子源(ESI+)在多反应监测(MRM)扫描模式下,超高效液相色谱-串联质谱(UPLC-MS-MS)测定蜂蜜中链霉素残留,并对仪器检测条件参数优化。结果方法线性范围为2.0μg/L^100μg/L;相关系数大于0.9998;检测限1.0μg/L;定量限2.0μg/L;3个不同水平标准添加回收率(n=7)为91.0%~100.5%;相对标准偏差(RSD)为4.2%~5.0%。结论方法操作简便、净化高效、准确、可靠、灵敏度高,在实际的测定中得到满意结果。
Objective To select the best operation parameters for determination of streptomycin in honey by solid phase extrac- tion coupled with ultra - high performance liquid chromatography - tandem mass spectrometry. Methods Samples were extrac- ted with EDTA - Na2 buffer solution and cleaned up on a strong cation exchange SPE column（ MCX）, separated on a HILIC col- umn （50 mm ×2.1 mm, 1. 7 μm） using acetonitrile -20 mmol/L ammonium acetate solution containing 0.1% formic acid as mobile phase for gradient elation. The analytes were detected in multiple reaction monitoring （MRM） mode via positive electros- pray ionization （ ESI ＋ ） and analyzed by UPLC/MS/MS. Results The detection limit of the method was 1.0 μg/L. LOQ was 2.0 μg/L. The linear range was 2.0 μg/L - 100 μg/L with the correlation coefficient above 0. 9998. The recoveries were 91.0% -100.5% （n = 7） and the RSD% was 4.2% -5.0%. Conclusion The method was simple, rapid and practical in determination of streptomycin in honey samples with satisfactory results.
出处
《中国卫生检验杂志》
北大核心
2014年第6期786-787,790,共3页
Chinese Journal of Health Laboratory Technology
关键词
固相萃取
超高效液相色谱-串联质谱
蜂蜜
链霉素
残留量
Solid phase extraction
Ultra- high performance liquid chromatography- tandem mass spectrometry
Honey
Streptomycin
Residues
