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岩白菜醇提物中岩白菜素类的降解动力学研究



全 文 :*基金项目:云南省教育厅科学研究基金项目(No.2010Y445)
 作者简介:魏泽英(1964~),女,云南人,硕士,副教授,主要从事物理化学和药物稳定性教学及科研工作,E-mail:janewei7@hot-
mail.com。
△通讯作者:李文军(1959~),女,云南人,副教授,主要从事中药化学和药物稳定性教学及科研工作,E-mail:lwj0699@qq.com。
岩白菜醇提物中岩白菜素类的降解动力学研究
魏泽英,孙海林,刘海周,李文军△
(云南中医学院,云南 昆明 650500)
  摘 要:目的:研究岩白菜醇提物中岩白菜素类的降解动
力学。方法:采用紫外分光光度法,考察在贮放阶段、浓缩工
序和干燥工序中岩白菜素类的含量变化,找出降解规律。结
果:岩白菜醇提液在室内常温下贮放20天,含量基本不变;岩
白菜醇提液在60℃浓缩时,降解符合一级反应动力学方程,降
解速率常数k=3.3×10-3 h-1,半衰期t1/2=210h=8.8d;岩
白菜醇提液随干燥温度升高、干燥时间加长降解率增大。结
论:岩白菜醇提液干燥温度不宜高,浓缩时间不宜长,以保证
最终药物的质量。
关键词:岩白菜;岩白菜素;醇提物;降解;动力学
中图分类号:R969.1 文献标识码:A
文章编号:1007-2349(2013)03-0052-02
岩白菜为虎耳草科岩白菜属植物岩白菜 Bergenia pur-
purascens(Hook.f.et Thoms.)Engl.的干燥根茎。岩白菜具
有多种作用,如:镇咳、抑菌、促进病变组织恢复的作用[1],增
强免疫、抗炎、抗氧化作用[2]等,现已广泛应用于临床。其中
主要有效成分岩白菜素是多元酚类化合物[3],该类化合物易
发生氧化、分解。由于岩白菜提取物在生产过程中普遍涉及
到贮放、浓缩和干燥,尚未见对岩白菜进行与本文相似研究的
文献报道,故重点对这三个阶段的岩白菜素类降解动力学进
行研究,为保证药品质量稳定提供参考。
1 仪器与材料
1.1 仪器 UV-2450紫外-可见分光光度计(日本岛津),
Precisa XS-125A型电子天平(瑞士),BUCHI-R-200旋转
蒸发仪(瑞士),SK3300LH超声清洗器(功率160W,上海汉克
科学仪器有限公司),数显恒温水浴锅(HH-6,国华电器有限
公司),电热鼓风干燥箱(DHG-9055A,上海一恒科技有限公
司)。
1.2 材料 岩白菜素对照品购于中国药品生物制品检定所;
岩白菜药材(同一批次)购于昆明菊花村药材市场,经云南中
医学院杨树德教授鉴定为虎耳草科岩白菜属植物岩白菜Ber-
genia purpurascens(Hook.f.et Thoms.)Engl.的干燥根茎;
D-101型大孔吸附树脂(天津农药股份有限公司树脂分公
司);去离子水。所有试剂均为分析纯。
2 方法与结果
2.1 对照品溶液的制备 精密称量3.1mg岩白菜素对照品
置于50mL 容量瓶中,加甲醇溶解,并定容至刻度,得到
62.00μg/mL的岩白菜素对照品溶液。
2.2 标准曲线的制备 精密吸取岩白菜素对照品溶液
(62.00μg/mL)1.3、2.2、3.1、4.0、4.9mL置10mL量瓶中,用
甲醇定容至刻度,以甲醇为空白对照,在274nm处测定吸收
度[4],以吸收度A为纵坐标,浓度c为横坐标进行线性回归分
析,得出标准曲线方程为 A=0.02347c+0.00534,相关系数
r=0.99992,表明岩白菜素对照品在8.06~30.38μg/mL浓度
范围内线性关系良好。
2.3 供试品溶液的制备[5] 取岩白菜药材粗粉适量,精密称
定,用50%乙醇加热回流提取3次,每次30min,溶媒用量为
药材10倍量。合并滤液,减压浓缩至乙醇回收完全,浓缩液
用去离子水补足至一定体积后,精密吸取等量溶液若干份,分
别进行贮放、浓缩和干燥处理,并经 D-101大孔吸附树脂纯
化后,取出适量置10mL容量瓶中,加甲醇定容至刻度,作为
测定岩白菜素含量的供试品溶液。
2.4 含量测定方法 取供试品溶液适量,以甲醇为空白对
照,于波长274nm处测定吸收度,按岩白菜素标准曲线回归方
程计算含量。
2.5 醇提液贮放阶段的降解动力学考察 精密吸取等量岩
白菜醇提液,置具塞三角瓶中,在室内常温下放置,间隔一定
时间取样品测定含量。结果见表1。
表1 贮放阶段的含量(n=6)
时间t(d) 岩白菜素类含量*(-c±s,mg/g)
0  109.98±0.34
5  110.13±0.57
10  110.06±0.38
15  110.17±0.87
20  109.87±0.45
  *含量均折算成药材标示含量
结果表明,岩白菜醇提液在室内常温下贮放20天,岩白
菜素类含量基本不变。
25 云 南 中 医 中 药 杂 志          2013年第34卷第3期
DOI:10.16254/j.cnki.53-1120/r.2013.03.037
2.6 醇提液浓缩阶段的降解动力学考察 精密吸取等量岩
白菜醇提液,置具塞三角瓶中,加去离子水适量,放置在60℃
水浴中加热,间隔一定时间取样品测定含量,结果见表2。
表2 浓缩工序的含量(n=6)
时间t(h) 岩白菜素类含量(-c±s,mg/g)
0  109.98±0.34
12  102.87±0.66
24  98.00±0.92
36  95.68±0.89
48  93.01±0.81
60  90.20±0.97
72  86.01±0.39
84  80.99±0.47
   经 回 归 分 析,得 回 归 方 程 lnc=4.6835-0.0033t
(r=-0.9901)。结果显示,岩白菜醇提液在60℃浓缩时,降
解动力学符合一级反应方程,降解速率常数k=3.3×10-3
h-1,半衰期t1/2=210h=8.8d。
2.7 醇提液干燥阶段的降解动力学考察 精密吸取等量岩
白菜醇提液,置具塞三角瓶中,分别置60℃、70℃、80℃和
90℃电热鼓风干燥箱中,间隔一定时间取样品测定含量。由
于随着温度升高、时间加长,样品的颜色加深,用吸收度不能
反映岩白菜素类物质的含量变化,故将其折算成透光率以反
映含量的变化,结果见表3和图1。
表3 干燥工序的透光率、降解率(n=6,%)
时间
t(h)
60℃ 70℃ 80℃ 90℃
透光率T 降解率 透光率T 降解率 透光率T 降解率 透光率T 降解率
0  32.6  0  32.6  0  32.6  0  32.6  0
12  28.7  12.0  28.1  13.8  27.3  16.3  26.0  20.2
24  27.2  16.6  27.0  17.2  26.8  17.8  25.4  22.1
36  24.7  24.2  25.1  23.0  24.8  23.9  23.3  28.8
48  24.5  24.8  24.1  26.1  23.7  27.3  22.7  30.4
60  23.9  26.7  23.1  29.1  22.7  30.4  21.2  35.0
  由于每个温度段的含量变化线性关系较差,无法用降解
动力学方程进行线性拟合,故采用降解率来反映岩白菜素类
的含量变化。结果显示:随着干燥温度升高、干燥时间加长,
岩白菜素类物质的降解率增大,60℃干燥降解较缓慢,90℃干
燥降解较迅速,90℃干燥60h降解率达35.0%。
图1 不同干燥温度透光率-时间图
3 小结与讨论
岩白菜醇提液中岩白菜素类60℃浓缩降解动力学符合一
级反应方程,干燥工序的降解线性关系差。岩白菜醇提液在
干燥、浓缩过程中,岩白菜素类成分均有一定程度的降解,且
随温度升高降解率增大,但在室内常温下贮放较稳定,提示温
度高对岩白菜醇提液中岩白菜素类成分的破坏严重。在实际
生产中,应尽量在较低温度下操作,并尽量缩短干燥、浓缩时
间。随干燥温度升高、干燥时间加长,样品颜色加深,可能是
由于高温、长时间加热导致的副反应产生了一些有色物质,相
关问题有待进一步研究。
参考文献:
[1]王刚,麻兵继 .岩白菜素的研究概况[J].安徽中医学院学报,
2002,21(6):59~62.
[2]阿斯亚,拜山佰,刘发,等 .岩白菜素的免疫增强作用[J].新疆医
学院学报,1998,21(3):189~193.
[3]云南省药物研究所 .云南重要天然药物[M].昆明:云南科技出版
社,2006:276~283.
[4]国家药典委员会 .中华人民共和国药典[S](一部).北京:中国医
药科技出版社,2010:384.
[5]刘海周,孙海林,李文军,等 .岩白菜中岩白菜素的纯化及提取工
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(收稿日期:2012-11-01
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殩殩


关 爱 生 命,预 防 艾 滋!
352013年第34卷第3期          云 南 中 医 中 药 杂 志
Yunnan Journal of Traditional Chinese Medicine and Materia Medica
Vol.34.No.3 (General No.237) March,2013
Main Content
Clinical Effect of Rhodiola Injection on the Treatment of Stable Angina Patients
   TANG Bin,WANG Zhi-xiang,LUO Qing-wen,et al………………………………………………………………………………………
Clinical Effect of Suhuang Cough Capsules Combined with Salmeterol Fluticasone on the Treatment of25Cough Variant Asthma Patients
   ZHU Ying-xia,LI Jin-run………………………………………………………………………………………………………………………
Study on the Antidepressant Activity and Preliminary Safety of Rose Powder
   LI Xiao-ying,QI Mei-feng,SONG Da,et al…………………………………………………………………………………………………
Study on the Degradation Kinetics of Bergenin Class in Bergenin Ethanol Extract
   WEI Ze-ying,SUN Hai-lin,LIU Hai-zhou,et al…………………………………………………………………………………………
Clinical Effect of Rhodiola Injection on the Treatment of Stable Angina Patients
TANG Bin,WANG Zhi-xiang,LUO Qing-wen,et al
(Yunnan Provincial Hospital of Traditional Chinese Medicine,Kunming Yunnan 650021)
Abstract:Objective:To observe the clinical effect of Rhodiola injection on the treatment of coronary heart disease patients with stable
angina pectoris.Methods:50patients were randomly divided into two groups.The control group was treated conventionaly with bed rest,
oxygen,aspirin enteric-coated tablets,nitrate preparations,beta blockers,statins and trimetazidine while the treatment group was added with
Rhodiola injection treatment besides the conventional treatment.The total effectiveness,the frequency and onset of angina pectoris attack,
blood rheology and electrocardiogram(ECG)of the two groups were compared after the treatment.Results:The total effectiveness of the
treatment group was higher than that of the control group,showing a statistical significance(P<0.05).Conclusion:Rhodiola injection has an
obvious therapeutic effect on the coronary heart disease patients with stable angina pectoris.
Key words:Rhodiola injection,stable angina pectoris,effectiveness
Clinical Effect of Suhuang Cough Capsules Combined with Salmeterol Fluticasone on the Treatment of 25Cough Variant Asthma Patients
ZHU Ying-xia,LI Jin-run
(The Third People's Hospital of Yunnan Province,Kunming Yunnan 650011)
Abstract:Objective:To observe the effect of Suhuang Cough Capsules on the treatment of cough variant asthma patients.Methods:50
patients were randomly divided into 2groups.The treatment group received 50ug/250ug of salmeterol fluticasone inhalation,once each
morning and evening,together with Suhuang Cough Capsules,three,three times a day oraly.The control group was only given 50ug/250ug
of salmeterol fluticasone inhalation,once each morning and evening.The clinical effectiveness and the lung function changes of the two groups
in four weeks were observed before and after the treatment.Results:The clinical effectiveness and the lung function of the patients in the two
groups improved after the treatment in varying degrees.The difference showed statistical significance(P<0.05).The effectiveness and the
lung function improvement of the treatment group were significantly better than that of the control group.Conclusion:The combination of
salmeterol fluticasone and Suhuang Cough Capsules has a better effect on the treatment of cough variant asthma patients.
Key words:Suhuang Cough Capsules,cough variant asthma,lung function
Study on the Antidepressant Activity and Preliminary Safety of Rose Powder
LI Xiao-ying,QI Mei-feng,SONG Da,et al
(Yunnan Colege of Traditional Chinese Medicine,KunmingYunnan 650200)
Abstract:Objective:To study the antidepressant activity and safety of rose powder.Methods:Depression experimental study was made by
using behavior despair models of swimming-forced mice and tail suspension mice to observe antidepressant activity;and acute toxicity mice and
subacute toxicity mice were used to examine its safety.Results:A10-day intragastrical administration for the mice with 0.25,0.5,1.0,2.0
g/kg of pure rose powder could significantly shorten the immobility time of the swimming-forced mice and the tail suspension mice.The
maximum dose administration for the mice by 8.0g/kg three times daily showed no significantly acute toxicity reaction.A 30-day
intragastrical administration for the mice with 1.0,2.0,4.0g/kg dose did not show significant change compared with that of the control group
in the coefficient of the other organs and serum AST,ALT,Cre,BUN,UA and also no deaths or visceral obvious abnormalities except for the
slow weight growth and the obvious lowering of the thymus and spleen coefficient of the high-dose group and BUN.Conclusion:The oraly
administrated mice showed significantly the antidepressant activity of the rose powder with their maximum tolerated dose of 2.0g/kg,and the
non-toxic dose of the continuous administration for 30days was 24.0g/kg.d.
Key words:rose powder,antidepressant,maximum tolerated dose,subacute toxicity;non-toxic dose
Study on the Degradation Kinetics of Bergenin Class in Bergenin Ethanol Extract
WEI Ze-ying,SUN Hai-lin,LIU Hai-zhou,et al
(Yunnan Colege of Traditional Chinese Medicine,Kunming Yunnan 650500)
Abstract:Objective:To study the degradation kinetics of Bergenin class in Bergenin ethanol extract.Methods:UV spectrophotometry was
used to investigate the content changes in the stage of its storage,concentrated process and dry process and find out its degradation law.
Results:When Bergenin alcohol extract was stored in room temperature for 20days,its content remained basicaly unchanged.Bergenin alcohol
extract concentrated at 60℃,the degradation accorded with first order reaction kinetics equation.The degradation rate constant was K=3.3
×10-3h-1,half-life was t1/2=210h=8.8d.Bergenin alcohol extract increased with drying temperature and longer drying time increased
degradation rate.Conclusion:Bergenin alcohol extract should not be in high drying temperature,with shorter concentrated time so as to
guarantee the quality of the final drug.
Key words:Bergenin,Bergenin,ethanol extract,degradation,kinetics