反相高效液相色谱法同时测定骨刺消痛胶囊中3种单酯型生物碱的含量  

Simultaneous determination of 3 monoester aconitum alkaloids in Guci Xiaotong capsules by RP-HPLC

作　　者：马云娜 徐远涛 焦洁 王国海 郭耀武[1,3] 杨海燕 MA Yun-na1, XU Yuan-tao3, JIAO Jie2, WANG Guo-hai2, GUO Yao-wu1,2., YANG Hai-yan2.(1. Shaanxi University of Chinese Medicine, Xianyang Shaanxi 712046; 2. Shaanxi Institute for Food and Drug Control, Xi＇ an 710065; 3. Shaanxi Duoyao Traditional Chinese Medicine Co., Ltd, Xianyang Shaanxi 71202)

机构地区：[1]陕西中医药大学,陕西咸阳712046 [2]陕西铎耀中药饮片有限公司,陕西咸阳712023 [3]陕西省食品药品监督检验研究院,西安710065

出　　处：《中南药学》2018年第3期412-415,共4页Central South Pharmacy

摘　　要：目的建立RP-HPLC法同时测定骨刺消痛胶囊中3种单酯型生物碱含量。方法色谱柱为Inert Sustain C18柱(5μm,4.6 mm×250 mm);流动相A为乙腈-四氢呋喃(25∶8),流动相B为0.1mol·L-1醋酸铵溶液(每1000 m L加冰醋酸0.5 m L),梯度洗脱;流速:1.0 m L·min-1;检测波长:234nm;柱温:30℃。结果苯甲酰新乌头原碱在进样量为0.0246~0.615μg与峰面积具有良好的线性关系(r=0.9997),低、中、高浓度平均加样回收率分别为96.8%、98.9%、97.8%,RSD分别为0.94%、0.88%、0.95%;苯甲酰乌头原碱在进样量为0.0987~2.4675μg与峰面积具有良好的线性关系(r=0.9999),低、中、高浓度平均加样回收率分别为100.1%、99.8%、100.3%,RSD分别为0.43%、0.25%、0.19%;苯甲酰次乌头原碱在进样量为0.0118~0.295μg与峰面积具有良好的线性关系(r=0.9998),低、中、高浓度平均加样回收率分别为97.7%、99.8%、98.1%,RSD分别为0.91%、1.2%、0.97%。结论本方法操作简便、灵敏度高、重复性好,结果准确,可作为骨刺消痛胶囊中单酯型生物碱的含量测定方法。Objective To establish an RP-HPLC method for the determination of the 3 monoester aconitum alkaloids in Guci Xiaotong capsules. Methods The determination was performed on Inert Sustain C18 chromatographic column （5 μm, 4.6 mm× 250 mm） with the mobile phase of A [acetonitrile-THF （25 ： 8）]-B [0.1 mol L-1 ammonium acetate solution （0.5 mL acetic acid added to the 1000 mL）] for gradient elution at the flow rate of 1.0 mL min-1. The detection wavelength was 234 nm and the column temperature was 30 ℃ . Results Benzoylmesaconine showed a good linearity at 0.0246 - 0.615 μg （r = 0.9997）, the average recoveries of low, middle and high concentration were 96.8%, 98.9% and 97.8%, and RSDs were 0.94%, 0.88% and 0.95%. Benzoylaconine showed a good linearity at 0.0987 - 2.4675 μg （r = 0.9999）, the average recoveries of low, middle and high concentration were 100.1%, 99.8% and 100.3%, and RSDs were 0.43%, 0.25% and 0.19%. Benzoylhypaconine showed a good linearity at 0.0118 - 0.295 μg （r = 0.9998）, the average recoveries of low, middle and high concentration were 97.7%, 99.8% and 98.1%, and RSDs were 0.91%, 1.2% and 0.97%. Conclusion This method is simple, sensitive, repeatable and accurate, which can be used for the determination of 3 monoester aconitum alkaloids in Guci Xiaotong capsules.

关 键 词：骨刺消痛胶囊 单酯型生物碱 苯甲酰新乌头原碱 苯甲酰乌头原碱 苯甲酰次乌头原碱 

分 类 号：R917[医药卫生—药物分析学]