
浏览全部资源
扫码关注微信
纸质出版日期:2020,
扫 描 看 全 文
薛巧如, 袁进烨, 丁刘洋, 等. UPLC法测定注射用特利加压素中有关物质的含量[J]. 中国药房, 2020,31(9).
XUE Qiaoru, YUAN Jinye, DING Liuyang, et al. Content Determination of Related Substances in Terlipressin for Injection by UPLC[J]. China Pharmacy, 2020,31(9).
目的:建立超高效液相色谱法(UPLC)法测定注射用特利加压素中有关物质的含量。方法:采用UPLC法测定5批注射用特利加压素制剂中有关物质的含量。色谱柱为XtimateUPLCC18,流动相A为硫酸铵缓冲液(pH2.3)-甲醇(90∶10,V/V),流动相B为硫酸铵缓冲液(pH2.3)-甲醇(60∶40,V/V),梯度洗脱,流速为0.2mL/min,检测波长为210nm,进样量为5μL。结果:注射用特利加压素中杂质A、B、C、D、F、H、I、K、L、N的检测质量浓度线性范围为0.43~3.86、0.44~3.95、0.44~3.97、0.45~4.08、0.45~4.05、0.50~4.50、0.47~4.26、0.47~4.23、0.46~4.13、0.44~3.96μg/mL(r≥0.9997);检测限分别为0.04、0.04、0.05、0.04、0.05、0.05、0.05、0.05、0.04μg/mL,定量限分别为0.13、0.13、0.14、0.13、0.15、0.14、0.14、0.14、0.13μg/mL;精密度、重复性、稳定性试验的RSD均小于8%;平均加样回收率分别为94.95%、97.81%、101.88%、95.26%、93.40%、102.48%、104.26%、102.31%、96.42%、90.42%,RSD%分别为1.89%、1.86%、0.68%、1.30%、1.98%、3.36%、1.26%、1.30%、1.19%、1.40%(n=9)。5批注射用特利加压素制剂中杂质总含量均小于4%。结论:建立的方法快速、简便、准确、专属性强,可用于注射用特利加压素中有关物质的定量分析。
OBJECTIVE:To establish UPLC method for the content determination of related substances in Terlipressin for injection. METHODS :UPLC method was used to determine the contents of related substances in 5 batches of Terlipressin for injection. The separation was performed on Xtimate UPLC C 18 column with mobile phase A consisted of ammonium sulfate buffer (pH 2.3)-methanol(90 ∶ 10,V/V)and mobile phase B consisted of ammonium sulfate buffer (pH 2.3)-methanol(60 ∶ 40,V/V) (gradient elution )at the flow rate of 0.2 mL/min. The detection wavelength was set at 210 nm,and sample size was 5 μL. RESULTS:The linear range of impurity A ,B,C,D,F,H,I,K,L and N were 0.43-3.86,0.44-3.95,0.44-3.97,0.45-4.08, 0.45-4.05,0.50-4.50,0.47-4.26,0.47-4.23,0.46-4.13,0.44-3.96 μg/mL(r≥0.999 7),respectively. The detection limits were 0.04, 0.04,0.05,0.04,0.05,0.05,0.05,0.05,0.04 μg/mL. The quantitation limits were 0.13,0.13,0.14,0.13,0.15,0.14,0.14, 0.14,0.13 μg/mL,respectively. RSDs of precision ,reproducibility and stability tests were all lower than 8%. The average recoveries were 94.95%,97.81%,101.88%,95.26%,93.40%,102.48%,104.26%,102.31%,96.42%,90.42%,with RSD s of 1.89%,1.86%,0.68%,1.30%,1.98%,3.36%,1.26%,1.30%,1.19%,1.40%(n=9),respectively. Total contents of impurities in 5 batches of Terlipressin for injection were all lower than 4%. CONCLUSIONS :Established method is rapid ,simple, accurate and specific ,which can be used for the quantitative analysis for related substances in Terlipressin for injection.
超高效液相色谱法注射用特利加压素有关物质含量测定
UPLCTerlipressin for injectionRelated substanceContent determination
0
浏览量
11
下载量
0
CSCD
关联资源
相关文章
相关作者
相关机构
公网安备50010302001817