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目的:建立HPLC法测定盐酸地芬尼多片中杂质烯化合物含量的方法。方法:采用岛津SHIMADAZU VP-ODS C_(18)色谱柱(250 mm×4.6 mm,5μm),以0.5%三乙胺溶液(用磷酸调pH至4.0)-甲醇(44:56)为流动相;流速为0.8 ml·min~(-1);检测波长为210 nm,柱温:30℃。结果:盐酸地芬尼多与杂质烯化合物及其他杂质完全分离,烯化合物的浓度在0.310～6.195μg·ml~(-1)范围内,与峰面积呈良好线性关系,r=0.999 9(n=7);最低检出限为1.24 ng,最低定量限为3.96 ng;低、中、高3种浓度的回收率分别为99.3%(RSD=0.6%)、99.2%(RSD=0.3%)、99.7%(RSD=0.3%)。结论:该方法操作简便、灵敏度高、结果准确,可用于盐酸地芬尼多片有关物质的检查中杂质烯化合物的含量测定。
OBJECTIVE: To establish a HPLC method for the determination of impurity alkene compounds in diltiazem hydrochloride tablets. METHODS: Shimadzu SHIMADAZU VP-ODS C 18 column (250 mm × 4.6 mm, 5 μm) was used as a mobile phase in a 0.5% triethylamine solution (adjusted to pH 4.0 with phosphoric acid) -methanol (44:56) ; Flow rate of 0.8 ml · min -1; detection wavelength of 210 nm, column temperature: 30 ℃. Results: Phenylephrine hydrochloride was completely separated from the other enantiomers and other impurities. The concentration of enkephalin was in the range of 0.310 ~ 6.195μg · ml ~ (-1) and showed a good linear relationship with the peak area, r = 0.999 9 (n = 7). The lowest detection limit was 1.24 ng and the lowest limit of quantification was 3.96 ng. The recoveries were 99.3% (RSD = 0.6%), 99.2% (RSD = 0.3%), 99.7% (RSD = 0.3%). Conclusion: The method is simple, sensitive, and accurate. It can be used to determine the content of impurity alkene compounds in the related substances of diphenhydramine hydrochloride tablets.