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目的:建立正相高效液相色谱法检测缬沙坦氢氯噻嗪片剂中缬沙坦对映异构体。方法:采用三(3,5-二甲基苯基氨基甲酸酯纤维素)涂覆多孔硅胶微球色谱柱(OD-H,250 mm×4.6 mm,5μm),以正己烷-异丙醇-三氟乙酸(75:25:0.1)为流动相,流速为0.8 mL·min~(-1),检测波长为230nm,进样量为10μL,柱温为25℃。结果:在上述色谱条件下缬沙坦与缬沙坦对映异构体可有效分离,分离度为2.8,缬沙坦对映异构体检测限为3 ng,定量限为10 ng,在1~50μg·mL~(-1)(r=0.999 8)浓度范围内线性关系良好。结论:本方法操作简单,灵敏度高,结果可靠,可作为缬沙坦氢氯噻嗪片中缬沙坦对映异构体的检查方法。
OBJECTIVE: To establish a method for the determination of valsartan enantiomers in valsartan hydrochlorothiazide tablets by normal-phase high performance liquid chromatography. METHODS: Porous silica microspheres (OD-H, 250 mm × 4.6 mm, 5 μm) were coated with tris (3,5-dimethylphenylcarbamate) - trifluoroacetic acid (75: 25: 0.1) as the mobile phase at a flow rate of 0.8 mL · min -1. The detection wavelength was 230 nm. The injection volume was 10 μL and the column temperature was 25 ℃. Results: Under the above chromatographic conditions, the enantiomers of valsartan and valsartan could be effectively separated with a resolution of 2.8, a limit of detection of 3 ng of the enantiomers of valsartan and a limit of quantification of 10 ng, ~ 50μg · mL -1 (r = 0.999 8) concentration range of good linear relationship. Conclusion: The method is simple, sensitive and reliable. It can be used as a method for the determination of valsartan enantiomers in valsartan hydrochlorothiazide tablets.