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[摘要]
目的 建立液质分析方法,对比收载于《中国药典》2015年版的同方不同剂型的枳术丸和枳术颗粒中20个活性成分的含量。方法 按《中国药典》2015年版制备工艺,采用3批原料制备枳术丸和枳术颗粒。建立高效液相色谱-三重四级杆-质谱(HPLC-QqQ-MS)分析2种剂型中20个活性成分含量的方法。色谱条件为Poroshell 120 SB-C18色谱柱(100 mm×4.6 mm,2.7 μm);流动相为0.1%甲酸水溶液(A)-0.1%甲酸乙腈溶液(B),梯度洗脱条件:0~7 min,23% B;7~17 min,23%~80% B;17~20 min,80%~100% B,20~30 min,100% B;体积流量0.5 mL/min;柱温30℃。结果 3批原料制备的枳术丸和枳术颗粒成品,20个活性成分的日服用量,丸剂是颗粒剂的1.48~13.37倍,总量相差493.01~615.07 mg。其中热不稳定性成分白术内酯I、白术内酯Ⅱ和白术内酯Ⅲ相差的倍数最大,其次为水溶性较差的川陈皮素。结论 枳术丸和枳术颗粒成品中活性成分含量有明显差异,尤其是处方中水溶性差、热不稳定的成分。
[Key word]
[Abstract]
Objective To comparative analyze the contents of 20 active ingredients in two dosage forms of Zhizhu Pills (ZP) and Zhizhu Granules (ZG).Methods Three batches of raw materials were used for the preparation of ZP and ZG according to the preparation process of China Pharmacopoeia (2015 Editon). Twenty active ingredients in the two dosage forms were detected simultaneously using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-QqQ-MS). The separation was performed on a Poroshell 120 SB-C18 (100 mm×4.6 mm, 2.7 μm) column with a flow rate of 0.5 mL/min. Mobile phase consisted of 0.1% formic acid in water (A)-0.1% formic acid in acetonitrile (B). The column temperature was set at 30℃. The gradient elution conditions:0-7 min, 23% B; 7-17 min, 23%-80% B; 17-20 min, 80%-100% B, 20-30 min, 100% B; flow rate was 0.5 mL/min.Results The contents of 20 active ingredients in the pills were 1.48-13.37 times that of the granules, the total difference of them perday were 493.02-615.08 mg.Conclusion There were significant differences in the content of active components in the two dosage forms of ZP and ZG, especially those components with poor solubility in water and thermal instability.
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[基金项目]
中央级公益性科研院所基本科研业务费专项资金(YZ-1655)