目的 探讨建立固相萃取-超高效液相色谱串联质谱法同时检测蜂蜜样品中氯霉素(CAP)和甲硝唑(MNZ)残留量的方法。方法 蜂蜜样品中氯霉素和甲硝唑采用优化的固相萃取方法提取,通过超高效液相色谱分离后,利用质谱正负离子切换模式同步测定合肥市本地25份蜂蜜样品中氯霉素和甲硝唑,以氘代同位素为内标,内标法定量,并分别添加低、中、高浓度标准液,测试精密度和回收率。结果 该方法线性良好,相关系数(r)>0.9992, 当取样量为5.0 g 时,氯霉素和甲硝唑的检出限(LOD)均为0. 001 μg/ kg,3种浓度水平的加标回收率和相对标准偏差(RSD)分别在93.6% ~ 105.0% 之间和2.2% ~7.6% 之间。结论 固相萃取-超高效液相色谱串联质谱法灵敏度高、重现性好,能满足蜂蜜样品中氯霉素和甲硝唑残留量的快速筛查与检测。
Abstract
Objective To establish a method for simultaneous determination of the chloramphenicol (CAP)and metronidazole (MNZ)in honey by a solid phase extraction coupled to ultra high performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS ). Methods CAP and MNZ in honey samples extracted by optimization of solid phase extraction method, then separated in UPLC, the 25 honey samples of Hefei local were simultaneous determined using mass spectrometry ESI- and ESI + mode and quantified by deuterated isotope internal standard method, also tested precision and recovery by adding low, medium and high concentration of standard solution. Results Good linear response were obtained from CAP and MNZ with the correlation coefficients(r) exceeding 0.9992. When sampling amount was 5.0 g, the limits of detection(LOD)or CAP and MNZ in honey were 0.001 μg/kg . The average recoveries at three spiked levels and the relative standard deviation( RSD) ranged from 93.6% to 105.0% and within 2.2% ~7.6%, respectively. Conclusion The method has advantages such as sensitive, accurate, reliable, and suitable for the analysis of quality and control method for trace CAP and MNZ in honey.
关键词
超高效液相色谱-串联质谱 /
固相萃取 /
氯霉素 /
甲硝唑 /
蜂蜜
Key words
UPLC-MS/MS /
Soild phase extraction /
Chloramphenicol /
Metronidazole /
Honey
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