摘要
目的:来曲唑原料药中1,2,4-三氮唑杂质的测定。方法:采用色谱柱ALLTIMA C18(4.6 mm×250 mm,5μm),流动相为乙腈-水进行梯度洗脱,紫外检测器,检测波长为200 nm,柱温:25℃,流速:1.0 m L/min。结果:杂质三氮唑在0.414 4~2.072 0μg/m L(r=0.999 2)范围内与峰面积线性关系良好,1,2,4-三氮唑的高、中、低浓度的平均回收率为102.3%,RSD为2.0%。结论:在该方法下,来曲唑与1,2,4-三氮唑能够得到有效分离,且该法准确性好、灵敏度高,适用于来曲唑原料药中三氮唑杂质的检测。
Objective:To establish a HPLC method to determine the triazole impurity in letrozole bulk drug.Methods:The reversed-phase HPLC analysis was carried out on an ALLTIMA C_(18) column(4.6 mm×250 mm,5μm)by gradient elution with a mobile phase consisting of acetonitrile–water(flow rate,1.0 mL/min;temperature,25℃).The UV detection wavelength was set at 200 nm.Results:The impurity(1H-1,2,4-triazole)were linear in the range of 0.4144~2.0720μg/mL(r=0.9992).The average recoveries of high,medium and low concentrations of triazole were 102.3%(RSD≤ 2.0%).Conclusion:The triazole could be eluted effectively via above method,which is specific,accurate and sensitive and is applicable for the determination of triazole impurity of letrozole API.
作者
常天歌
朱建
吴文营
郑威
毕路夜
赵冬梅
杨秀丽
曹志凌
Chang Tiange;Zhu Jian;Wu Wenying;Zheng Wei;Bi Luye;Zhao Dongmei;Yang Xiuli;Cao Zhiling(Jiangsu Ocean University,Lianyungang 222005,China;Lianyungang Guike Pharmaceutical,Lianyungang 222000,China)
出处
《山东化工》
CAS
2022年第9期114-116,共3页
Shandong Chemical Industry
基金
江苏省产学研合作项目(BY2020579)
江苏省研究生科研与实践创新项目(SJCX20-1232、SJCX20-1220、SJCX20-1225)。
