HPLC法测定氨氯地平氢氯噻嗪缬沙坦片中的有关物质
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篇名: HPLC法测定氨氯地平氢氯噻嗪缬沙坦片中的有关物质
TITLE:
摘要: 目的:建立测定氨氯地平氢氯噻嗪缬沙坦片中有关物质的方法。方法 :采用高效液相色谱法。色谱柱为Symmetry C18,流动相为[水-乙腈-三氟乙酸(90 ∶ 10 ∶ 0.1,V/V/V)]-[水-乙腈-三氟乙酸(10 ∶ 90 ∶ 0.1,V/V/V)](梯度洗脱),流速为0.6 mL/min,检测波长为237 nm(杂质A)和225 nm(杂质B、C、D),柱温为30 ℃。结果:杂质A、B、C、D检测质量浓度线性范围分别为93.43~987.34 ng/mL(r=0.999 4)、12.27~255.92 ng/mL(r=0.999 6)、78.96~657.17 ng/mL(r=0.999 9)、28.39~218.16 ng/mL(r=0.999 7);定量限分别为91.27、11.35、78.31、26.56 ng,检测限分别为22.98、3.13、19.17、8.16 ng;精密度的RSD<2.0%,稳定性、重复性试验中只检出杂质A,RSD=0.79%;回收率分别为99.4%~100.6%(RSD=0.41%,n=9)、98.9%~102.0%(RSD=1.04%,n=9)、99.4%~100.9%(RSD=0.56%,n=9)、98.6%~101.2%(RSD=0.92%,n=9)。结论:该方法简便、快速、灵敏、重复性好,可用于测定氨氯地平氢氯噻嗪缬沙坦片中的有关物质。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of related substances in Amlodipine hydrochlorothiazide and valsartan tablets. METHODS: HPLC method was used. The determination was performed on Symmetry C18 column with mobile phase consisted of water-acetonitrile-trifluoroacetic acid (90 ∶ 10 ∶ 0.1,V/V/V) and water-acetonitrile-trifluoroacetic(10 ∶ 90 ∶ 0.1,V/V/V)(gradient elution) at the flow rate of 0.6 mL/min. The detection wavelength was set at 237 nm (impurity A) and 225 nm (impurity B, C, D). The column temperature was 30 ℃. RESULTS: The linear range of impurity A, B, C, D were 93.43-987.34 ng/mL (r=0.999 4),12.27-255.92 ng/mL(r=0.999 6), 78.96-657.17 ng/mL(r=0.999 9), 28.39-218.16 ng/mL(r=0.999 7), respectively. The limits of quantitation were 91.27, 11.35, 78.31, 26.56 ng; the limits of stability and detection were 22.98, 3.13, 19.17, 8.16 ng. RSDs of precision tests were lower than 2.0%. Only impurity A was found in repeatability test,RSD=0.79%. Recoveries were 99.4%-100.6%(RSD=0.41%,n=9),98.9%-102.0%(RSD=1.04%,n=9),99.4%-100.9%(RSD=0.56%,n=9), 98.6%-101.2%(RSD=0.92%,n=9), respectively. CONCLUSIONS: The method is simple, rapid, sensitive and repeatable, and can be used for the determination of related substance in Amlodipine hydrochlorothiazide and valsartan tablets.
期刊: 2017年第28卷第12期
作者: 李亚萍,王静,周立新,陆步实
AUTHORS: LI Yaping,WANG Jing,ZHOU Lixin,LU Bushi
关键字: 氨氯地平;氢氯噻嗪;缬沙坦;有关物质;高效液相色谱法;氨氯地平氢氯噻嗪缬沙坦片
KEYWORDS: Amlodipine; Hydrochlorothiazide; Valsartan; Related susbtance; HPLC; Amlodipine hydrochlorothiazide and valsartan tablets
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