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作 者:郭娅 王文婷 袁林 GUO Ya;WANG Wenting;YUAN Lin(Wanzhou Institute for Food and Drug Control, Chongqing, China 404000)
出 处:《中国药业》2019年第3期39-41,共3页China Pharmaceuticals
摘 要:目的建立同时测定舒筋活血片中4-甲氧基水杨醛、羟基红花黄色素A、原儿茶酸、α-香附酮和山柰素含量的高效液相色谱(HPLC)法。方法色谱柱采用Agilent Eclipse XDB-C18柱(250 mm×4. 6 mm,5μm),流动相为0. 7%醋酸溶液(A)-甲醇(B)[梯度洗脱(0~13 min,30%A,70%B; 13~25 min,30%A→80%A,70%B→20%B; 25~40 min,80%A,20%B)],检测波长为254 nm,流速为1. 0 m L/min,柱温为30℃,进样量为10μL。结果 4-甲氧基水杨醛线性范围为1. 92~95. 76μg/mL(r=0. 999 7),平均回收率为100. 39%,RSD为1. 05%(n=6);α-香附酮线性范围为4. 22~210. 90μg/m L(r=0. 999 8),平均回收率为98. 61%,RSD为1. 00%(n=6);原儿茶酸线性范围为2. 15~107. 30μg/mL(r=0. 999 7),平均回收率为98. 84%,RSD为1. 39%(n=6);羟基红花黄色素A线性范围为2. 34~117. 00μg/m L(r=0. 999 6),平均回收率为100. 43%,RSD为0. 50%(n=6);山柰素线性范围为0. 83~41. 44μg/mL(r=0. 999 8),平均回收率为99. 20%,RSD为1. 64%(n=6)。结论该方法准确,重复性好,简单易行,可用于舒筋活血片的质量控制。Objective To establish an HPLC method for simultaneous determination of 4-methoxysalicylaldehyde,hydroxysafflor yellow A,protocatechuic acid, α-cyperone and kaempferide in Shujin Huoxue Tablets. Methods The chromatographic column was Agilent Eclipse XDB-C18 column( 250 mm × 4. 6 mm,5 μm),the mobile phase was 0. 7% acetic acid solution( A)-methanol( B) [ gradient elution( 0-13 min,30% A,70% B. 13-25 min,30% A→80% A,70% B→20% B. 25-40 min,80% A,20% B) ],the detection wavelength was 254 nm, the flow rate was 1. 0 mL/min,the column temperature was 30 ℃, and the simple size was 10 μL. Results The linear concentration range of 4-methoxysalicylaldehyde was 1. 92-95. 76 μg/mL( r = 0. 999 7),the average recovery rate was 100. 39%,and RSD was 1. 05( n = 6). The linear concentration range of α-cyperone was 4. 22-210. 90 μg/mL( r = 0. 999 8), the average recovery rate was 98. 61%, and RSD was 1. 00( n = 6). The linear concentration range of protocatechuic acid was 2. 15-107. 30 μg/mL( r =0. 999 7),the average recovery rate was 98. 84%,and RSD was 1. 39( n = 6). The linear concentration range of hydroxysafflor yellow A was 2. 34-117. 00 μg/mL( r = 0. 999 6),the average recovery rate was 100. 43%,and RSD was 0. 50( n = 6). The linear concentration range of kaempferide was 0. 83-41. 44 μg/mL( r = 0. 999 8),the average recovery rate was 99. 20%,and RSD was 1. 64( n = 6).Conclusion The method is accurate,reproducible and simple,which can be used for the quality control of Shujin Huoxue Tablets.
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