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目的建立高效液相色谱法测定佐匹克隆的有关物质。方法高效液相色谱法采用Apollo C18(250mm×4.6mm,5μm)柱分离,流动相以8.1g/L十二烷基硫酸钠,1.6g/L磷酸二氢钠水溶液(用10%磷酸调pH3.5)-乙腈(60:40),流速1.2ml.min-1,检测波长303nm,柱温30℃。结果高效液相色谱测定佐匹克隆在2.0~79.0ng(Y=2280977.80X+784.96r,=0.9999)及2-氨基-5-氯吡啶在2.0~79.0ng(Y=1757411.68X-60.63r,=1.0000)范围内线性关系良好。佐匹克隆的最低检出量为0.05ng,2-氨基-5-氯吡啶的最低检出量为0.10ng;2-氨基-5-氯吡啶、各破坏性分解产物能和主峰分离;高、中、低3种浓度的加样回收率分别为101.25%(RSD=0.42%)、101.24%(RSD=0.62%)和101.11%(RSD=0.19%);稳定性试验表明样品不稳定,需要新鲜配制。结论建立高效液相色谱法测定佐匹克隆显示准确、灵敏、可靠、专属性强,可用于佐匹克隆的质量控制。
Objective To establish a HPLC method for the determination of zopiclone. Methods High performance liquid chromatography with Apollo C18 (250 mm × 4.6 mm, 5 μm) column was used. The mobile phase consisted of 8.1 g / L sodium dodecyl sulfate, 1.6 g / L aqueous sodium dihydrogen phosphate solution (adjusted to pH3 with 10% phosphoric acid .5) -acetonitrile (60:40) at a flow rate of 1.2 ml.min-1 at a detection wavelength of 303 nm at a column temperature of 30 ° C. Results The determination of zopiclone by HPLC was in the range of 2.0 ~ 79.0ng (Y = 2280977.80X + 784.96r, = 0.9999) and 2.0 ~ 79.0ng (Y = 1757411.68X-60.63r, 1.0000) within a good linear relationship. The detection limit of zopiclone was 0.05 ng, the detection limit of 2-amino-5-chloropyridine was 0.10 ng, and the destructive decomposition products of 2-amino-5-chloropyridine could separate from the main peak. The recovery rates of medium and low concentrations were 101.25% (RSD = 0.42%), 101.24% (RSD = 0.62%) and 101.11% (RSD = 0.19%) respectively. The stability test showed that the sample was unstable and required fresh Preparation. Conclusion The HPLC method for the determination of zopiclocin is accurate, sensitive, reliable and specific. It can be used for the quality control of zopiclone.