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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。
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.
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
AmlodipineHydrochlorothiazideValsartanRelated susbtanceHPLCAmlodipine hydrochlorothiazide and valsartan tablets
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