摘要
目的建立富马酸喹硫平片中有关物质的HPLC测定法。方法采用HPLC法测定富马酸喹硫平片中KL-Imp01、KL-Imp02、KL-Imp03、KL-Imp04、KL-Imp05杂质含量。色谱柱为Techmate C18柱(250 mm×4.6 mm×5μm),以甲醇-水-三乙胺(磷酸调pH至8.0)(670:330:4)为流动相,流速为1.0 mL/min,柱温为40℃,检测波长为250 nm,进样体积为20μL。结果在该色谱条件下,可同时检测到5个杂质,各杂质与富马酸喹硫平的分离度均大于1.5。KL-Imp01、KL-Imp02、KL-Imp03、KL-Imp04、KL-Imp05定量限分别为0.1451μg/mL、0.0388μg/mL、0.1133μg/mL、0.0493μg/mL、0.0510μg/mL,检测限分别为0.0435μg/mL、0.0117μg/mL、0.0340μg/mL、0.0148μg/mL、0.0153μg/mL,线性范围分别为0.1451~0.9673μg/mL、0.0388~0.9710μg/mL、0.1133~0.7554μg/mL、0.0493~0.8213μg/mL、0.0510~0.8196μg/mL。各杂质在48 h内溶液稳定性良好,峰面积RSD<2.0%(n=8)。低、中、高三个浓度的加样回收率为92.10%~108.00%(n=3)。结论该方法简便、灵敏、重现性和耐用性好,能够用于富马酸喹硫平片的质量控制。
Objective To establish a HPLC method for the determination of related substances in quetiapine fumarate tablets.Methods The impurity content of KL-Imp01,KL-Imp02,KL-Imp03,KL-Imp04,KL-Imp05 in Quetiapine fumarate tablets was determiened by HPLC.An HPLC method was adopted with Techmate C18 column(250 mm4.6 mm5μm).The mobile phase was methanol-water-triethylamine(phosphoric acid adjusted pH to 8.0)(670:330:4).The flow rate was 1.0 mL/min.The column temperature was 40℃.The detection wavelength is 250 nm.The injection volume was 20μL.Results Under this chromatographic condition,5 impurities(KL-Imp01、KL-Imp02、KL-Imp03、KL-Imp04、KL-Imp05)can be detected at the same time,and each impurity is well separated from the principal component,and the separation degree is greater than 1.5.The limits of quantitation were 0.1451μg/mL,0.0388μg/mL,0.1133μg/mL,0.0493μg/mL,0.0510μg/mL;the limits of detection were 0.0435μg/mL,0.0117μg/mL,0.0340μg/mL,0.0148μg/mL,0.0153μg/mL The linear ranges of them were 0.1451~0.9673μg/mL,0.0388~0.9710μg/mL,0.1133~0.7554μg/mL,0.0493~0.8213μg/mL,0.0510~0.8196μg/mL.The solution stability of the impurities was good within 48 h,and the RSD of the peak area was less than 2.0%(n=8).The average recovery of low,medium and high recovery solutions was 92.1~108.0%(n=3).Conclusion The method is simple,sensitive,reproducible and durable,and can be used for the quality control of quetiapine fumarate tablets.
作者
张雪梅
孙鑫
陆荣政
刘荣华
ZHANG Xuemei;SUN Xin;LU Rongzheng;LIU Ronghua(School of Pharmacy,Jiangxi University of Chinese Medicine,Jiangxi,Nanchang 330004,China;Nanjing Zenkom Pharmaceutical Co.,LTD,Jiangsu,Nanjin 210038)
出处
《江西医药》
CAS
2024年第2期155-159,共5页
Jiangxi Medical Journal
