HPLC波长切换法同时测定九味双解口服液中5种成分的含量

Simultaneous Determination of 5 Components in Jiuweishuangjie Oral Liquid by HPLC with Wavelength Switching

目的:建立HPLC波长切换法同时测定九味双解口服液中绿原酸、咖啡酸、木犀草苷、黄芩苷和大黄素的含量。方法:采用Shiseido Capcell Pak C_(18)(200 mm×4.6 mm,5μm)色谱柱,流动相为甲醇(A)-0.1%磷酸溶液(B)(梯度洗脱),流速为1.0 ml·min^(-1),柱温为25℃,检测波长(0~19 min,在327 nm波长下检测绿原酸;19~25 min,在323 nm波长下检测咖啡酸;25~35 min,在350 nm波长下检测木犀草苷;35~55 min,在320 nm波长下检测黄芩苷;55~60 min,在254 nm波长下检测大黄素)。结果:绿原酸、咖啡酸、木犀草苷、黄芩苷和大黄素的线性范围分别为0.34~6.81μg·ml^(-1)(r=0.999 9)、0.23~4.56μg·ml^(-1)(r=0.999 5)、1.32~26.38μg·ml^(-1)(r=0.999 9)、9.60~192.01μg·ml^(-1)(r=0.999 9)、1.14~22.80μg·ml^(-1)(r=0.999 6);平均加样回收率分别为99.50%(RSD=0.52%)、99.10%(RSD=1.43%)、98.83%(RSD=0.94%)、99.98%(RSD=0.21%)、99.22%(RSD=0.82%)(n=9)。结论:本文建立的含量测定方法,具有操作简便、结果准确、重现性良好的特点,可用于九味双解口服液的质量控制。

Objective： To establish a method for the simultaneous determination of chlorogenic acid, coffee acid, luteolin-7-O-glu- coside, baicalin and emodin in Jiuweishuangjie oral hquid by an HPLC wavelength switching method. Methods： A Shiseido Capcell Pak C18 column （200 mm×4.6 mm,5μm） was used with the mobile phase of methanol-0. 1% phosphoric acid solution （gradient elution） at a flow rate of 1.0ml·min^-1, the column temperature was 25~C, the detection wavelength was changed as follows： 0-19 min, 327 nm for chlorogenic acid; 19-25min, 323 nm for coffee acid; 25-35 rain, 350 nm for luteolin-7-O-glucoside; 35-55 min, 320 nm for baicalin; 55-60 rain, 254 nm for emodin. Results： The linear range was 0.34-6.81μg·mil （r =0.999 9） for chlorogenic acid, 0. 23-4. 56μg·ml^-1（r = 0.999 5 ） for coffee acid, 1.32-26.38 μg·ml^-1（ r = 0.999 9） for luteolin-7-O-glucoside, 9.60-192.01 μg·ml^-1 （ r = 0. 999 9） for baicalin and 1.14-22.80μg·ml^-1（ r = 0.999 6） for emodin; the average of recovery was 99.50% （RSD = 0.52%）,99.10% （RSD-1.43%）,98.83% （RSD=0.94%）, 99.98% （RSD=0.21%） and99.22%（RSD=0. 82%）（n= 9）, respectively. Conclusion ： The determination method has the advantages of simple operation, accurate results and good reproduc-ibility, which can be used for the quality control of Jiuweishuangiie oral liquid.