高效液相色谱法测定缬沙坦氢氯噻嗪片中缬沙坦对映异构体

Determination of valsartan enantiomer in compound valsartan and hydrochlorothiazide tablets by HPLC

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 an HPLC method for determination of valsartan enantiomers in compound valsartan and hydrochlorothiazide tablets. Methods： HPLC analysis was performed at 25 ℃ on a three （3, 5-two methyl phenyl carbamate cellulose） column （OD-H, 250 mm × 4.6 mm,5 μm） coated with porous silica microspheres eluted with a mobile phase containing n-hexane-isopropanol-trifluoro acid （ volume ratio, 75：25 ： 0.1 ） in the elution at a flow rate of 0.8 mL·min^ -1. The UV detection was set at 230 nm. Results： Under the established chromatographic conditions, valsartan and valsartan enantiomers were well separated. The resolution between valsartan and valsartan enantiomers was 2.8, and the LOD and LOQ were 3 ng and 10 ng, respectively. The linear range of detection limit for valsartan enantiomers was 1 - 50 μg· mL^- 1 （ r = 0. 999 8 ）. Conclusion ： The method is sensitive, specific and accurate with a good repeatability, and can be used for measuring the enantiomers of vatsartan in compound valsartan and hydrochlorothiazide tablets.