HPLC波长切换法同时测定女金丸中12种成分

Simultaneous Determination of Twelve Constituents in Nüjin Pills by HPLC Combined with Wavelength Switching

目的建立同时测定女金丸中芍药苷、甘草苷、阿魏酸、芸香柚皮苷、橙皮苷、黄芩苷、汉黄芩苷、桂皮醛、黄芩素、丹皮酚、甘草酸铵和汉黄芩素12种成分的HPLC方法。方法采用Agilent Eclipse plus C18(4. 6 mm×250 mm,5μm)色谱柱,乙腈(A)-0. 2%甲酸溶液(B)为流动相,梯度洗脱(0~25 min,10%~35%A; 25~37 min,35%~59%A; 37~40 min,59%~75%A),柱温和流速分别为30℃和1 m L·min-1,波长切换,0~20 min,230 nm; 20~40 min,270 nm。结果 12种成分实现完全分离,并与其他成分均能达到良好的分离;芍药苷、甘草苷、阿魏酸、芸香柚皮苷、橙皮苷、黄芩苷、汉黄芩苷、桂皮醛、黄芩素、丹皮酚、甘草酸铵和汉黄芩素分别在0. 011~1. 062、0. 002~0. 237、0. 003~0. 259、0. 006~0. 641、0. 029~2. 925、0. 033~3. 339、0. 008~0. 834、0. 003~0. 258、0. 008~0. 772、0. 008~0. 824、0. 007~0. 724和0. 005~0. 539μg进样量范围内,与色谱峰峰面积呈良好线性响应;平均回收率(n=6)分别为99. 3%、98. 4%、99. 1%、99. 4%、99. 5%、99. 6%、99. 4%、99. 2%、99. 0%、99. 6%、99. 1%和99. 4%; RSD分别为0. 35%、1. 02%、0. 33%、0. 38%、0. 18%、0. 27%、0. 40%、0. 74%、0. 53%、0. 16%、0. 08%和0. 21%。结论本方法操作简便,测定结果准确,可用于女金丸的质量控制。

OBJECTIVE To establish an HPLC method for simultaneous determination of 12 constituents in Nujin pills. METH- ODS The analysis was carried out on Agilent Eclipse plus Cls column（4. 6 mm× 250 mm,5 μm）, using a mobile phase of acetonitrile （A）-0. 2% formic acid solution （B） by a gradient elution program （0- 25 min, 10% -35% A; 25- 37 min, 35% -59% A; 37 -40 min, 59% -75% A） at a flow rate of 1 mL · min -1 at 30 %. The detection wavelength was set at 230 nm in the first 20 min, and then changed to 270 nm between 20 and 40 min. RESULTS The linear ranges of paeoniflorin, liquiritin, ferulicacid, narirutin, aurantiamarin, baicalin, wogonoside, cinnam aldehyde, baicalein, paeonol, ammonium glycyrrhetate and wogonin fell within the ranges of 0.011- 1.062 μg, 0.002-0.237 μg, 0.003 -0.259 μg, 0.006-0.641 μg, 0.029-2.925 μg, 0.033 -3.339 μg, 0. 008 - 0. 834 μg, 0. 003 - 0. 258 μg, 0. 008 - 0. 772 μg, 0. 008 - 0. 824 μg, 0. 007 - 0. 724 μg and 0. 005 - 0. 539 μg, respectively. The recoveries were 99.3%, 98.4%, 99. 1%, 99.4%, 99.5%, 99.6%, 99.4%, 99.2%, 99.0%, 99.6%, 99. 1%, and 99. 4%, respectively. The relative standard deviations were 0. 35%, 1.02%, 0. 33%, 0. 38%, 0. 18%, 0. 27%, 0. 40%, 0. 74%, 0. 53% , 0. 16% , 0. 08% and 0. 21% , respectively （n =6）. CONCLUSION This method is simple, accurate and convenient for the quality control of Nujin pills.