HPLC法同时测定小儿清咽颗粒中5种成分的含量
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篇名: HPLC法同时测定小儿清咽颗粒中5种成分的含量
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摘要: 目的:建立同时测定小儿清咽颗粒中哈巴苷、哈巴俄苷、绿原酸、咖啡酸、连翘苷含量的方法。方法:采用高效液相色谱法。色谱柱为Zorbax SB-C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为210 nm(0~13 min,哈巴苷)、327 nm(13~25 min,绿原酸、咖啡酸)、277 nm(25~29 min,连翘苷)、210 nm(29~40 min,哈巴俄苷),柱温为30 ℃,进样量为10 μL。结果:哈巴苷、哈巴俄苷、绿原酸、咖啡酸、连翘苷检测进样量线性范围分别为8.400~168.0 ng(r=0.999 6)、11.30~226.0 ng(r=0.999 8)、128.8~257.6 ng(r=0.999 3)、8.110~162.2 ng(r=0.999 6)、29.69~593.8 ng(r=0.999 4);定量限分别为33.39 、451.2、515.2 、324.5、1 188 ng/mL,检测限分别为8.348、112.8、128.8、81.12 、297.0 ng/mL;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为96.39%~98.64%(RSD=0.83%,n=6)、96.60%~98.89%(RSD=0.89%,n=6)、96.28%~99.22%(RSD=1.25%,n=6)、96.49%~99.54%(RSD=1.16%,n=6)、96.26%~99.70%(RSD=1.30%,n=6)。结论:该方法操作简单、结果准确,适用于小儿清咽颗粒中5种成分含量的同时测定。
ABSTRACT: OBJECTIVE: To develop a method for simultaneous determination of harpagide, harpagoside, chlorogenic acid, caffeic acid and phillyrin in Xiaoer qingyan granules. METHODS: HPLC method was adopted. The determination was performed on Zorbax SB-C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (gradient elution) at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm (0-13 min, harpagide), 327 nm (13-25 min, chlorogenic acid and caffeic acid), 277 nm (25-29 min, phillyrin), 210 nm (29-40 min, harpagosid); the column temperature was 30℃, and sample size was 10 μL. RESULTS: The linear ranges of harpagide, harpagosid, chlorogenic acid, caffeic acid and phillyrin were 8.400-168.0 ng(r=0.999 6),11.30-226.0 ng (r=0.999 8), 128.8-257.6 ng (r=0.999 3), 8.110-162.2 ng(r=0.999 6),29.69-593.8 ng(r=0.999 4), respectively. LOQs of the 5 components were 33.39, 451.2, 515.2, 324.5, 1 188  ng/mL; LODs were 8.348, 112.8, 128.8, 81.12, 297.0 ng/mL, respectively; RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The recoveries were 96.39%-98.64%(RSD=0.83%,n=6), 96.60%-98.89%(RSD=0.89%,n=6), 96.28%-99.22%(RSD=1.25%,n=6), 96.49%-99.54%(RSD=1.16%,n=6), 96.26%-99.70%(RSD=1.30%,n=6), respectively. CONCLUSIONS: The method is simple, accurate and suitable for simultaneous determination of 5 components in Xiaoer qingyan granules
期刊: 2017年第28卷第21期
作者: 张申亮,聂黎行
AUTHORS: ZHANG Shenliang,NIE Lixing
关键字: 小儿清咽颗粒;高效液相色谱法;波长切换;哈巴苷;哈巴俄苷;绿原酸;咖啡酸;连翘苷
KEYWORDS: Xiaoer qingyan granules; HPLC; Wavelength switching; Harpagide; Harpagosid; Chlorogenic acid; Caffeic acid; Phillyrin
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