摘要
建立高效液相色谱测定4-甲氧基-4-甲基哌啶盐酸盐衍生后含量的方法。样品经4-硝基苯甲酰氯衍生后,采用Agilent EC-C18色谱柱(4.6 mm×150 mm, 4μm),以0.01 mol/L的磷酸二氢铵溶液-乙腈(67∶33)为流动相,流速1.0 mL/min,检测波长为210 nm,进样体积为10μL,柱温35℃,外标法定量。结果表明,该方法重复性以及中间精密度良好,在0.024 16~0.144 96 mg/mL浓度范围内线性关系良好,相关系数(r)大于0.999,方法检出限为0.048μg/mL,定量限为0.120μg/mL,样品溶液在室温放置12 h稳定性良好,当检测条件发生微小变化时检测结果无明显变化,耐用性良好。该方法操作简便、准确有效,适合4-甲氧基-4-甲基哌啶盐酸盐的定量检测。
A high performance liquid chromatographic(HPLC)method was established for determination of 4-methoxy-4-methylpiperidine hydrochloride after derivatization.The sample was derived by 4-nitrobenzoyl chloride.Chromatographic separation was achieved on an Agilent EC-C 18(4.6 mm×150 mm,4μm),using 0.01 mol/L ammonium dihydrogen phosphate in water and acetonitrile as mobile phase at a flow rate of 1.0 mL/min,and the wavelengths at 210 nm,and the column temperature was set as 35℃,and the external standard method was used for quantification.The results showed that 4-methoxy-4-methylpiperidine hydrochloride after derivatization had good repeatability and intermediate precision,it had good linearities in the range of 0.02416~0.14496 mg/mL,with correlation coefficients(r)greater than 0.999.The detection limit of the method was 0.048μg/mL and the quantitation limit of the method was 0.120μg/mL.Sample solution was stable at room temperature for 12 h.It had good robustness.The results indicated that the method was simple,accurate and reliable,and was suitable for the quantitative detection of 4-methoxy-4-methylpiperidine hydrochloride.
作者
张秀晶
孙小芬
闫园园
易克会
ZHANG Xiu-jing;SUN Xiao-fen;YAN Yuan-yuan;YI Ke-hui(TransThera Sciences(Nanjing),Inc.,Jiangsu Nanjing 210032,China)
出处
《广州化工》
CAS
2024年第18期111-113,共3页
GuangZhou Chemical Industry
