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目的建立固相萃取-超高效液相色谱-串联质谱法同时检测消毒产品中的4种抗生素(氯霉素、甲砜霉素、氟甲砜霉素和甲硝唑)。方法样品经40 mmol/L盐酸溶液提取,MCS固相萃取柱富集净化,乙酸乙酯洗脱氯霉素类抗生素,5%氨水甲醇洗脱甲硝唑,超高效液相色谱-串联质谱仪进行分析。结果标准物质在0 ng/ml~5.0 ng/ml时,方法的线性关系较好,相关系数(r)≥0.998;方法的检出限为0.003 ng/ml~0.01 ng/ml,定量限为0.01 ng/ml~0.02 ng/ml;4种抗生素的加标浓度为0.187 5 ng/ml~0.875 ng/ml时,回收率为70.40%~121.96%,相对标准偏差(RSD)为1.61%~9.30%。在10份消毒产品的检测中,检测到甲硝唑的存在,阳性检出率为20%。结论该方法的灵敏度高、选择性好、操作简单,适用于消毒产品中氯霉素、甲砜霉素、氟甲砜霉素和甲硝唑的同时检测。
Objective To establish a simultaneous determination of four antibiotics (chloramphenicol, thiamphenicol, florfenicol and metronidazole) in disinfection products by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 40 mmol / L hydrochloric acid solution, the MCS solid phase extraction column was enriched for purification, the chloramphenicol was eluted with ethyl acetate, the metronidazole was eluted with 5% ammonia methanol, the mass spectrometry was performed with ultra performance liquid chromatography-tandem mass spectrometry Analyze. Results The linearity of the method was good at 0 ng / ml ~ 5.0 ng / ml with the correlation coefficient (r) ≥0.998. The detection limit was 0.003 ng / ml ~ 0.01 ng / ml and the limit of quantification was 0.01 The recoveries ranged from 70.40% to 121.96% and the relative standard deviations (RSDs) ranged from 1.61% to 9.30% with spiked concentrations ranging from 0.187 5 ng / ml to 0.875 ng / . Metronidazole was detected in 10 samples of disinfection products. The positive detection rate was 20%. Conclusion The method has high sensitivity, good selectivity and simple operation. It is suitable for the simultaneous detection of chloramphenicol, thiamphenicol, florfenicol and metronidazole in disinfection products.