摘要
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 develop a method for simultaneous determination of chloramphenicol,thiamphenicol,florfenicol and metronidazole in disinfection products by ultra-performance liquid chromatography tandem mass spectrum（ UPLC-MS / MS）after enrichment and purification with MCS-SPE column. Methods The products was extract by 40 mmol / L hydrochloric acid solution,enriched and purified by MCS-SPE column,then,the target chemicals were eluted with ethyl acetate and metronidazole with 5% ammonia-methanol solution,the analysts were analyzed with UPLC-MS. Results The linearity was good when the subjects were among 0. 0 ng / ml-5. 0 ng / ml. The correlation coefficients（ r） were all ≥0. 998,the limits of quantification and detection（ LODs） were respectively 0. 01 ng / ml-0. 02 ng / m L,0. 003 ng / ml-0. 01 ng / ml. The recoveries of the 4antibiotics were in the range of 70. 40%-121. 96%,and the relative standard deviations（ RSDs） were among 1. 61%-9. 30%,when the standard concentration of the 4 antibiotics were among 0. 187 5 ng / ml-0. 875 ng / ml. Ten disinfection products were detected by this method,and metronidazole were detected in two samples with the positive rate of 20%. Conclusion This method is simple,sensitive,selective and accurate,and can be applied for simultaneous detection of chloramphenicol,thiamphenicol,florfenicol and metronidazole in disinfection products.
出处
《中国卫生检验杂志》
CAS
2015年第23期4015-4018,共4页
Chinese Journal of Health Laboratory Technology
关键词
超高效液相色谱-串联质谱
消毒产品
抗生素
Ultra-performance liquid chromatography tandem mass spectrum
Disinfection products
Antibiotic
