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

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， 5 μm），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0.050~0.297 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），0.012~0.071μg（r=0.999 6），0.023~0.138 μg（r=0.999 9），0.016~0.094 μg（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 simultaneous 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 also be used as the standard for the quality control of Fuke Fenqing pills.

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