摘要
建立高效液相色谱法测定来曲唑起始物料4-氟苯腈中的有关物质。采用Inertsil ODS-3(4.6 mm×250 mm,5μm)色谱柱,以0.01 mol/L磷酸氢二钾缓冲溶液(磷酸调pH=5.5)-乙腈(V∶V=60∶40)为流动相进行等度洗脱,流速1.0 mL/min,柱温25℃,进样量20μL,检测波长225 nm。4-氟苯腈与杂质峰间分离度大于2.0。4-氟苯腈及各杂质在各自浓度范围内线性关系良好(r≥0.999 7),检测限0.003 8~0.033 0μg/mL,定量限0.025~0.099μg/mL,杂质平均回收率96.01%~102.22%。方法专属性强,灵敏度高,准确度好,满足来曲唑起始物料4-氟苯腈中有关物质检测要求。
To establish a HPLC method for the determination of the related substances in 4-fluorobenzonitrile as the starting materials of Letrozole.An Inertsil ODS-3 column(4.6 mmx250 mm,5μm)was adopted with DAD detecter.The mobile phase was 0.01 mol/L dipotassium hydrogen phosphate buffer(pH=5.5)-acetonitrile(V:V=60:40)at flow rate of 1.0 mL/min.The detection wavelength was set at 225 nm,the injection volume was 20μL and the column temperature was 25 C.The resolution between 4-fluorobenzonitrile and rejacent peaks was more than 2.0.4-Fluorobenzonitrile and each impurity within their respective concentration and peak aera showed a good linearity(r≥0.9997),the limit of detection was 0.0038~0.0330μg/mL;the limit of quantification was 0.025~0.099μg/mL,the average recovery rate was 96.01%~102.22%.This method has good specificity,high accuracy and sensitivity,which is suitable for the determination of the related substances in 4-fluorobenzonitrile.
作者
邢雪敏
张锡霞
李欣
刘梦瑶
刘葵葵
张琳
XING Xue-min;ZHANG Xi-xia;LI Xin;LIU Meng-yao;LIU Kui-kui;HANG Lin(Shandong Academy of Pharmaceutical Sciences,Ji'nan 250101,China;Key Laboratory for Chemical Drugs of Shandong Province,Ji'nan 250101,China;Shandong Freda Pharmaceutical Group Co.,Ltd.,Ji'nan 250101,China;Shandong Provincial Key Laboratory of Mucosa and Transdermal Drug Delivery Technology,Ji'nan 250101,China)
出处
《精细化工中间体》
CAS
2023年第5期78-81,共4页
Fine Chemical Intermediates
