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目的建立脱氢环氧甲基醌霉素(DHMEQ)起始原料2,5-二甲氧基苯胺的有关物质和含量测定方法。方法采用C_(18)柱(250 mm×4.6 mm,5μm)为固定相,以乙腈-0.05%磷酸(15∶85)为流动相;检测波长为295 nm;流速为1 m L·min~(-1);柱温为25℃。结果空白溶剂无干扰;在0.08~0.12 mg·mL~(-1)范围内,线性回归方程为y=10 971 361.177 1x+29 634.000 0,相关系数为0.999 7;3个浓度(80%、100%、120%)平均回收率分别为98.6%、100.7%、101.0%,RSD为1.2%(n=9)。结论该方法简便、灵敏度好、可靠性高,可用于DHMEQ起始原料2,5-二甲氧基苯胺的有关物质和含量测定。
OBJECTIVE To establish a method for the determination of related substances and contents of 2, 5-dimethoxyaniline, the starting material for dehydrocycline methylquinidine (DHMEQ). Methods The mobile phase consisted of C_ (18) column (250 mm × 4.6 mm, 5 μm) with acetonitrile-0.05% phosphoric acid (15:85) as the mobile phase. The detection wavelength was 295 nm and the flow rate was 1 m L · min ~ -1); column temperature is 25 ℃. Results The blank solvent had no interference. The linear regression equation was y = 10 971 361.177 1x + 29 634.000 0 in the range of 0.08-0.12 mg · mL -1 with a correlation coefficient of 0.999 7. The three concentrations (80%, 100 %, 120%), the average recoveries were 98.6%, 100.7% and 101.0%, respectively. The RSD was 1.2% (n = 9). Conclusion The method is simple, sensitive, and highly reliable. It can be used to determine the related substances and contents of 2,5-dimethoxyaniline, the starting material of DHMEQ.