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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
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)
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
Fuke Fenqing pills
genipin 1-gentiobioside
geniposide
peoniflorin
glycyrrhizic acid
ferulic acid
calceolarioside B
berberine
hgustrazine
Chinese patent medicine standard improvement
HPLC
wavelength conversion
