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 C_(18),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 m L/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/m L(r=0.999 4)、12.27~255.92 ng/m L(r=0.999 6)、78.96~657.17 ng/m L(r=0.999 9)、28.39~218.16 ng/m L(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 hydrochlo- rothiazide and valsartan tablets, METHODS： HPLC method was used. The determination was performed on Symmetry C18 colmun with mobile phase consisted of water-acetonitrile-trifluoroacetic acid （90： 10：0.1, V/V/V） and water-acetonitrile-trifluoroacetie（ 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 rig. 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% （P,SD=0.41%, n=9）, 98.9% -102.0% （P, SD=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.
出处
《中国药房》
CAS
北大核心
2017年第12期1714-1717,共4页
China Pharmacy
