Xu Juan, Chen Jie, Shao Linzhi, Li Xun
Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China.
Se Pu. 2011 May;29(5):450-3. doi: 10.3724/sp.j.1123.2011.00450.
A method for the simultaneous determination of metronidazole, tinidazole, ornidazole, ronidazole and dimetridazole in oral hygiene by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed. The sample was diluted with 0.1% formic acid/acetonitrile (95:5, v/v), then centrifuged and filtered with a membrane. The separation was carried out on a Cloversil C18 column (100 mm x 2.1 mm, 3.5 microm) with the gradient elution of 0.1% formic acid and acetonitrile as the mobile phases. The analytes were determined by UPLC-MS/MS and quantified by external standard method. The calibration curves showed good linearity in the range of 1.0-60.0 microg/L with r > or = 0.9992. The recoveries were 91.5%-108% at the three spiked levels of 10.0, 20.0 and 100 mg/kg, and the relative standard deviations were 1.14%-5.22%. This method is easy, sensitive and suitable for the determination of nitroimidazoles in oral hygiene.
建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定口腔卫生用品中甲硝唑、替硝唑、奥硝唑、罗硝唑和地美硝唑的方法。样品用0.1%甲酸/乙腈(95:5,v/v)稀释,然后离心并用滤膜过滤。采用Cloversil C18柱(100 mm×2.1 mm,3.5μm)进行分离,以0.1%甲酸和乙腈为流动相进行梯度洗脱。通过UPLC-MS/MS测定分析物,并采用外标法进行定量。校准曲线在1.0 - 60.0μg/L范围内呈良好线性,r≥0.9992。在10.0、20.0和100 mg/kg三个加标水平下回收率为91.5% - 108%,相对标准偏差为1.14% - 5.22%。该方法简便、灵敏,适用于口腔卫生用品中硝基咪唑类的测定。