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
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篇名: 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
TITLE:
摘要: 目的:建立同时测定复方罗布麻片Ⅰ中维生素B1、硫酸双肼屈嗪、维生素B6、维生素B5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 C18,流动相为乙腈-0.2%磷酸溶液(梯度洗脱),流速为0.5 mL/min,检测波长为285 nm(维生素B1、硫酸双肼屈嗪、维生素B6)、210 nm(维生素B5),柱温为30 ℃,进样量为10 μL。结果:维生素B1、硫酸双肼屈嗪、维生素B6、维生素B5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、22.72~113.6 μg/mL(r均为0.999 9);定量限分别为0.267、0.274、0.062、0.124   μg/mL,检测限分别为0.095、0.088、0.021、0.039 μg/mL;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B1、硫酸双肼屈嗪、维生素B6、维生素B5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。
ABSTRACT: 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 10 μL. RESULTS: The linear ranges of vitamin B1, dihydralazine sulfate, vitamin B6 and vitamin B5 were 41.66-208.3 μg/mL (r=0.999 9), 127.0-635.0 μg/mL (r=0.999 9), 40.74-203.7 μg/mL (r=0.999 9) and 22.72-113.6 μg/mL (r=0.999 9), respectively. The limits of quantitation were 0.267, 0.274, 0.062, 0.124 μg/mL, respectively. The limits of detection were 0.095, 0.088, 0.021, 0.039 μg/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.
期刊: 2018年第29卷第5期
作者: 徐硕,金鹏飞
AUTHORS: XU Shuo,JIN Pengfei
关键字: 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
KEYWORDS: HPLC; Compound Apocynum venetum tabletsⅠ; Vitamin B1; Dihydralazine sulfate; Vitamin B6; Vitamin B5; Content
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