HPLC法同时测定复方罗布麻片Ⅰ中硫酸双肼屈嗪和3种维生素的含量  

Simultaneous Determination of Dihydralazine Sulfate and Three Vitamins in Compound Apocynum venetum Tablets Ⅰ by HPLC

作　　者：徐硕[1] 金鹏飞[1] XU Shuo;JIN Pengfei(Dept.of Pharmacy,Beijing Hospital/National Center of Gerontology/Beijing Key Lab of Drug Clinical Risk and Personalized Medication Evaluation,Beijing 100730,China)

机构地区：[1]北京医院药学部/国家老年医学中心/药物临床风险与个体化应用评价北京市重点实验室,北京100730

出　　处：《中国药房》2018年第5期607-610,共4页China Pharmacy

基　　金：国家自然科学基金青年科学基金项目(No.81303216);北京医院"科技新星"项目(No.BJ-2016-039)

摘　　要：目的:建立同时测定复方罗布麻片Ⅰ中维生素B_1、硫酸双肼屈嗪、维生素B_6、维生素B_5含量的方法。方法:采用高效液相色谱法对2家企业共8批次样品进行含量测定。色谱柱为Waters XBridge C_(18),流动相为乙腈-0.2%磷酸溶液(梯度洗脱),流速为0.5 m L/min,检测波长为285 nm(维生素B_1、硫酸双肼屈嗪、维生素B_6)、210 nm(维生素B_5),柱温为30℃,进样量为10μL。结果:维生素B_1、硫酸双肼屈嗪、维生素B_6、维生素B_5检测质量浓度线性范围分别为41.66~208.3、127.0~635.0、40.74~203.7、22.72~113.6μg/m L(r均为0.999 9);定量限分别为0.267、0.274、0.062、0.124μg/m L,检测限分别为0.095、0.088、0.021、0.039μg/m L;精密度、稳定性、重复性试验的RSD均<2.0%(n=6);平均加样回收率分别为98.70%(RSD=0.69%,n=9)、99.74%(RSD=1.2%,n=9)、99.89%(RSD=1.0%,n=9)、99.25%(RSD=1.2%,n=9)。测定的8批样品中,维生素B_1、硫酸双肼屈嗪、维生素B_6、维生素B_5含量分别为标示量的91.44%~98.74%、36.68%~95.23%、92.42%~97.90%、91.36%~99.48%,其中硫酸双肼屈嗪的含量差异较大,最低值与最高值间相差2.6倍。结论:该方法准确可靠、操作简便,可用于同时测定复方罗布麻片Ⅰ中上述4种成分的含量。OBJECTIVE:To establish a method for simultaneous determination of vitamin B1,dihydralazine sulfate,vitamin B6 and vitamin B5 in Compound Apocynum venetum tabletsⅠ.METHODS:HPLC method was used for content determination of 8 batches of samples from 2 enterprises.The determination was performed on Waters XBridge C18 column with mobile phase consisted of acetonitrile-0.2%phosphoric acid(gradient elution)at the flow rate of 0.5 mL/min.The detection wavelengths were set at 285 nm(vitamin B1,dihydralazine sulfate,vitamin B6)and 210 nm(vitamin B5).The column temperature was 30℃,and sample size was 10μL.RESULTS:The linear ranges of vitamin B1,dihydralazine sulfate,vitamin B6 and vitamin B5 were 41.66-208.3μg/mL(r=0.999 9),127.0-635.0μg/mL(r=0.999 9),40.74-203.7μg/mL(r=0.999 9)and 22.72-113.6μg/mL(r=0.999 9),respectively.The limits of quantitation were 0.267,0.274,0.062,0.124μg/mL,respectively.The limits of detection were 0.095,0.088,0.021,0.039μg/mL,respectively.RSDs of precision,stability and reproducibility tests were all lower than 2.0%(n=6).The average recoveries were 98.70%(RSD=0.69%,n=9),99.74%(RSD=1.2%,n=9),99.89%(RSD=1.0%,n=9),99.25%(RSD=1.2%,n=9),respectively.Among 8 batches of samples,the contents of vitamin B1,dihydralazine sulfate,vitamin B6 and vitamin B5 were 91.44%-98.74%,36.68%-95.23%,92.42%-97.90%,91.36%-99.48%of labelled amount,respectively.The contents of dihydralazine sulfate were significantly different and differed by 2.6 times between the lowest and the highest threshold value.CONCLUSIONS:The method is accurate,reliable,simple and can be used for simultaneous determination of the above 4 components in Compound A.venetum tabletsⅠ.

关 键 词：高效液相色谱法 复方罗布麻片Ⅰ 维生素B1 硫酸双肼屈嗪 维生素B6 维生素B5 含量 

分 类 号：R927.2[医药卫生—药学]