[關鍵詞]
[摘要]
目的 利用高效液相色譜聯(lián)合電噴霧檢測器(HPLC-CAD),建立同時測定小建中合劑中芍藥內(nèi)酯苷、芍藥苷、甘草苷、甘草酸、桂皮醛及6-姜辣素含量的檢測方法,并對小建中合劑穩(wěn)定性進行研究。方法 采用Thermo Hypersil GOLD C18色譜柱(250 mm×4.6 mm,5 μm),以80%乙腈(A)-10 mmol·L-1甲酸銨(甲酸調(diào)pH值至4.0)(B)為流動相,梯度洗脫,體積流量1.0 mL·min-1,柱溫35℃,CAD霧化器溫度為35℃,過濾常數(shù)為5.0,采集頻率為10 Hz,進樣量20 μL。同時測定小建中合劑在加速及長期試驗下各成分含量的變化。結(jié)果 各成分分離度均良好,陰性無干擾;芍藥內(nèi)酯苷、芍藥苷、甘草苷、甘草酸、桂皮醛及6-姜辣素的線性范圍分別為2.01~40.16、4.21~84.20、1.18~23.64、0.60~12.04、0.70~14.06及1.30~25.90 μg·mL-1(r≥0.999 1);平均加樣回收率(n=6)為97.55%~98.46%,RSD≤3.0%。穩(wěn)定性研究結(jié)果表明,芍藥內(nèi)酯苷、芍藥苷、甘草苷、桂皮醛及6-姜辣素在加速條件下各成分質(zhì)量濃度有明顯下降,提示本品種不宜在高溫下長時間放置。結(jié)論 經(jīng)方法學驗證,建立的HPLC-CAD法具有良好的靈敏度及準確度,為小建中合劑的全面質(zhì)量控制提供科學依據(jù),本品應置陰涼處貯藏。
[Key word]
[Abstract]
Objective To develop an HPLC-CAD method for simultaneous determination of six active ingredients of albiflorin, paeoniflorin, liquiritin, glycyrrhizic acid, cinnamaldehyde and 6-gingerol in Xiaojianzhong Mixture. Methods The chromatographic separation was performed on a Thermo Hypersil GOLD C18 column (250 mm×4.6 mm, 5 μm) with 80% acetonitrile (A)-10 mmol·L-1 ammonium acetate (formic acid tone pH 4.0) (B) as the mobile phase for gradient elution, the flow rate was 1.0 mL·min-1, the column temperature was maintained at 35℃, the nebulization temperature of detector was 35℃, the filtration constant was 5.0, the acquisition frequency was 10 Hz, and injection volume was 20 μL. At the same time, the content changes of each component of Xiaojianzhong Mixture under accelerated and long-term test were determined to provide a basis for the stability and storage conditions of the variety. Results The separation of each component was good, negative and no interference. The linear ranges of albiflorin, paeoniflorin, liquiritin, glycyrrhizic acid, cinnamaldehyde and 6-gingerol were 2.01-40.16, 4.21-84.20, 1.18-23.64, 0.60-12.04, 0.70-14.06 and 1.30-25.90 μg·mL-1 (r ≥ 0.999 1), respectively. The average recoveries were 97.55%-98.46%, and the RSD ≤ 3.0%.The results of stability investigation showed that the contents of albiflorin, paeoniflorin, liquiritin, glycyrrhizic acid, cinnamaldehyde and 6-gingerol decreased rapidly under accelerated condition, implied that the storage time of Xiaojianzhong Mixture under high temperature condition should not be too long. Conclusion The method is sensitive and accurate by method validation, which can be used for the overall assessment of the quality of Xiaojianzhong Mixture, this variety should be stored in a cool place.
[中圖分類號]
R284.1
[基金項目]