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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 the simultaneous determination of eight components (genipin gentiobioside, geniposide, paeoniflorin, glycyrrhizic acid, ferulic acid, aliskiren B, berberine and ligustrazine) method. METHODS: DIKMA Platisil ODS column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile (A) and 0.1% phosphoric acid solution (B) % A → 16% A; 20-30 min, 16% A → 40% A; 30-50 min, 40% A → 80% A) at a flow rate of 1 mL · min -1. (240 nm, genipin gentianobioside, geniposide, paeoniflorin, glycyrrhizin; 327 nm, ferulic acid, aliskiren B, berberine; 295 nm, ligustrazine). Results: The linear range of genipin gentian, geniposide, paeoniflorin, glycyrrhizic acid, ferulic acid, apiridin, berberine and tetramethylpyrazine were 0.050 ~ 0.297μg (r = 0.999 (R = 0.999 9), 0.030 ~ 0.180 μg (r = 0.999 7), 0.024 ~ 0.146 μg (r = 0.999 9), 0.012 ~ 0.071 μg The average recoveries were 97.0% (RSD = 1.8%), 98.3% (RSD = 1.2) and the average recoveries were 0.023 ~ 0.138μg (r = 0.999 9) and 0.016 ~ 0.094μg (RSD = 1.5%), 97.6% (RSD = 1.5%), 97.0% (RSD = 1.9%), 98.4% (RSD = 1.5%). The contents of Genipin gentiobioside, Geniposide, Paeoniflorin, Glycyrrhizic acid, Ferulic acid, Alopecter B, Berberine and ligustrazine in three batches of samples were 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. Conclusion: The method can be used to determine the contents of gentiancinanidase gentianobioside, geniposide, paeoniflorin, glycyrrhizin, ferulic acid, o-phenyletin glycoside B, berberine and ligustrazine, which can be used as gynecology An effective way to clarify the quality control of pills.