基于高效液相色谱-二极管阵列检测法测定妇科分清丸中8个成分的含量  

Simultaneous determination of eight compounds in Fuke Fenqing pills by HPLC-DAD

作　　者：郝乘仪[1] 冯波[1] 郭淑英[1] 朱鹤云[1] 昌盛[1] 

机构地区：[1]吉林医药学院药学院药物分析教研室,吉林132013

出　　处：《药物分析杂志》2017年第5期803-811,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：吉林市科技局资助项目(20165020)

摘　　要：目的:建立同时测定妇科分清丸中8个成分(京尼平龙胆双糖苷、栀子苷、芍药苷、甘草酸、阿魏酸、木通苯乙醇苷B、小檗碱、川芎嗪)的方法。方法:采用DIKMA Platisil ODS色谱柱(250 mm×4.6 mm,5μm),柱温30℃,流动相为乙腈(A)-0.1%磷酸水溶液(B),采用梯度洗脱(0~20 min,10%A→16%A;20~30 min,16%A→40%A;30~50 min,40%A→80%A),流速为1 mL·min^(-1),,变换波长检测(240 nm,京尼平龙胆双糖苷、栀子苷、芍药苷、甘草酸;327 nm,阿魏酸、木通苯乙醇苷B、小檗碱;295 nm,川芎嗪)。结果:京尼平龙胆双糖苷、栀子苷、芍药苷、甘草酸、阿魏酸、木通苯乙醇苷B、小檗碱、川芎嗪的线性范围分别为0.050~0.297μg(r=0.999 6),0.125~0.750μg(r=0.999 9),0.029~0.176μg(r=0.999 5),0.030~0.180μg(r=0.999 7),0.024~0.146μg(r=0.999 9),0.012~0.071μg(r=0.999 6),0.023~0.138μg(r=0.999 9),0.016~0.094μg(r=0.999 8),平均回收率分别为97.0%(RSD=1.8%)、98.3%(RSD=1.2%)、100.7%(RSD=1.5%)、98.6%(RSD=1.5%)、97.0%(RSD=1.9%)、98.4%(RSD=1.8%)、97.9%(RSD=1.5%)、107.7%(RSD=1.5%);3批样品中京尼平龙胆双糖苷、栀子苷、芍药苷、甘草酸、阿魏酸、木通苯乙醇苷B、小檗碱、川芎嗪的含量分别为0.130~0.131、0.588~0.589、0.158~0.164、0.130~0.135、0.043~0.045、0.052~0.059、0.170~0.171、0.042~0.050 mg·g^(-1)。结论:该法能测定妇科分清丸京尼平龙胆双糖苷、栀子苷、芍药苷、甘草酸、阿魏酸、木通苯乙醇苷B、小檗碱、川芎嗪的含量,可作为妇科分清丸质量控制的一个有效的方法。Objective： To establish a method for simuhaneous determination of genipin 1-gentiobioside, geniposide, peoniflorin, glycyrrhizic acid, ferulic acid, calceolarioside B, berberine and ligustrazine in Fuke Fenqing pills.Methods： The separation was performed on a DIKMA Platisil ODS column （ 250 mm × 4.6 mm, 5 μm ） with gradient elution using acetonitrile and 0.1% phosphoric acid solution as mobile phase. The flow rate was 1 mL· min-1 and the detection wavelengths were 240 nm for genipin 1-gentiobioside, geniposide, peoniflorin and glycyrrhizic acid, and 327 nm for ferulic acid, calceolarioside B and berberine, and 295 nm for ligustrazine, respectively. Results： The linear ranges of genipin 1-gentiobioside, geniposide, peoniflorin, glycyrrhizic acid, ferulic acid, calceolarioside B, berberine and ligustrazine were 0.050-0.297 μg （ r=-0.999 6 ）, 0.125-0.750 μg （ r=-0.999 9 ）, 0.029-0.176 μg （ r=0.999 5 ）, 0.030-0.180 μg（ r=0.999 7 ）, 0.024-0.146 μg（ r=0.999 9 ）, 0.012-0.071 μg（ r=0.999 6 ）, 0.023-0.138 μg （ r=0.999 9 ）and 0.016-0.094 μg （ r=0.999 8 ）, respectively. Their average recoveries were 97.0% （ RSD=1.8% ）, 98.3% （ RSD=1.2% ）, 100.7% （ RSD=1.5% ）, 98.6% （ RSD=1.5% ）, 97.0% （ RSD=1.9% ）, 98.4% （ RSD=1.8% ）, 97.9% （ RSD=1.5% ） and 107.7% （ RSD=1.5% ）. The contents of genipin 1-gentiobioside, geniposide, peoniflorin, glycyrrhizic acid, ferulic acid, calceolarioside B, berberine and ligustrazine in three samples were 0.130-0.131 mg· g-1, 0.588-0.589 mg· g-1, 0.158-0.164 mg· g-1, 0.130-0.135 mg· g-1, 0.043-0.045 mg· g-1, 0.052-0.059 mg· g-1, 0.170- 0.171 mg· g-1 and 0.042-0.050 mg· g-1, respectively. Conclusion： The HPLC method established can be used to determine the contents of genipin 1-gentiobioside, geniposide, peoniflorin, glycyrrhizic acid, ferulic, calceolarioside B, berberine and ligustrazine in Fuke Fenqing pills. The method can akso be used as the standard for the quality control of Fuke Fenqing pills.

关 键 词：妇科分清丸 京尼平龙胆双糖苷 栀子苷 芍药苷 甘草酸 阿魏酸 木通苯乙醇苷B 小檗碱 川芎嗪 中成药标准提高 高效液相色谱 变换波长 

分 类 号：R917[医药卫生—药物分析学]