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目的建立同时测定消毒产品中甲硝唑、盐酸金霉素、土霉素二水合物、盐酸米诺环素、红霉素及盐酸四环素的高效液相色谱-串联质谱(LC-MS/MS)检测方法。方法样品经甲醇超声提取,0.45μm聚四氟乙烯膜过滤后,选择WatersSymmetryC18(2.1mm×150mm,3.5μm)为分析柱,5mmol/L乙酸铵缓冲溶液、甲醇和乙腈为流动相,用LC-MS/MS正离子扫描多反应监测模式检测。结果上述6种抗生素在0～2000ng/ml范围内线性关系良好,相关系数均大于0.998,回收率为74.7%～114%,相对标准偏差为1.6%～20.2%。该法成功用于115件皮肤、黏膜使用的膏霜剂型抗(抑)菌制剂消毒产品中抗生素残留量的检测。结论该法操作简单,灵敏度高,选择性强,可用于膏霜剂型消毒产品中抗生素残留量的测定。
OBJECTIVE To establish a method for the simultaneous determination of metronidazole, chlortetracycline hydrochloride, oxytetracycline dihydrate, minocycline hydrochloride, erythromycin and tetracycline hydrochloride in sterile products by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) Detection method. Methods After the sample was extracted by methanol and filtered through 0.45μm PTFE membrane, Waters SymmetryC18 (2.1mm × 150mm, 3.5μm) was used as analytical column, 5mmol / L ammonium acetate buffer solution, methanol and acetonitrile as mobile phase, LC-MS / MS positive ion scan multi-reaction monitoring mode detection. Results The above six antibiotics had a good linearity in the range of 0-2000ng / ml, the correlation coefficient was higher than 0.998, the recovery was 74.7% ~ 114% and the relative standard deviation was 1.6% ~ 20.2%. The method was successfully applied to the detection of antibiotic residues in disinfectant products for 115 skin and mucous membrane anti-bacterial preparations. Conclusion The method is simple, sensitive and selective. It can be used for the determination of antibiotic residues in cream-type disinfection products.