肝康颗粒说明书（精选7篇）
篇1：肝康颗粒说明书
【通用名称】肝康颗粒
【商品名称】肝康颗粒
【拼音全码】GanKangKeLi
【主要成份】柴胡、田基黄、茵陈、蒲公英、甘草、金钱草。
【性状】肝康颗粒为淡棕色或棕色的颗粒;气香，味苦。
【适应症/功能主治】清肝利湿。用于肝湿热所致的黄疸，症见周身，小便俱黄，体疲乏力，纳呆，恶心厌油，苔黄腻，脉弦滑数;及急慢性肝炎、胆囊炎。
【规格型号】10g*10袋
【用法用量】口服，一次1袋，一日2次，小儿酌减或遵医嘱。
【不良反应】尚不明确。
【禁忌】尚不明确。
【注意事项】尚不明确。
【药物相互作用】如与其他药物同时使用可能会发生药物相互作用详情请咨询医师或药师。
【贮藏】密封。
【包装】每盒10小袋，每小袋10g。
【有效期】18月
【批准文号】国药准字Z3444
【生产企业】吉林省华威药业有限公司
肝康颗粒(华威)的功效与作用肝康颗粒(华威)清肝利湿。用于肝湿热所致的黄疸，症见周身，小 便俱黄，体疲乏力，纳呆，恶心厌油，苔黄腻，脉 弦滑数;及急慢性肝炎、胆囊炎。
肝康颗粒服用常见问题
肝功能是多方面而且非常复杂的。其病因复杂，肝功能出现问题给患者们带来很大的影响，大大降低了他们的生活质量。而肝康颗粒在市面上被广泛应用，那么，肝康颗粒对肝功能的恢复有作用吗?
肝康颗粒对肝功能的恢复有作用，肝康颗粒对慢性乙型肝炎患者的呕吐、恶心、纳差、黄疸及脘腹痞胀的复常率均有较好的效果。对肝功能的恢复亦有明显作用，退黄疸优于乙肝宁冲剂等护肝药，说明肝康颗粒有明显改善慢性乙肝患者的症状体征，保护肝脏的作用。慢性病毒性乙型肝炎见湿热症侯者多表现为正虚邪恋，虚实夹杂，正气虚弱，邪毒内伏，病情迁延难愈，且以湿热中阻为多，该组方辨证立方，随症施治，肝康颗粒一方面清热、利湿、化淤和解毒以祛邪;另一方面在健脾、养肝和益肾以匡正，祛邪不忘扶正，从而达到标本兼治。
肝康颗粒的主要成份有柴胡、田基黄、茵陈、蒲公英、甘草、金钱草等。清肝利湿、解毒化淤、养血利肝。具有抗病毒和保肝降酶的双重作用，用于利胆湿热所致的黄疸，症见周身，小便俱黄，体疲乏力，纳呆，恶心厌油，苔黄腻，脉弦滑数;及急慢性肝炎，迁延性肝炎及胆囊炎。未见任何毒副作用及不良反应。作用也称副反应，系指应用治疗量的药物后所出现的治疗目的以外的药理作用。药物正作用是主要的.一种药物常有多方面的作用，既有治疗目的的作用也并存有非治疗目的的作用。副作用和治疗作用在一定条件下是可以转化的，治疗目的的不同，也导致副作用的概念上的转变。副作用常为一过性的，随治疗作用的消失而消失。但是有时候也可引起后遗症。
篇2：肝康颗粒说明书
【商品名称】利肝康片(东方草)
【拼音全码】LiGanKangPian(DongFangCao)
【主要成份】主要成份为青叶胆总苷。
【性状】利肝康片(东方草)为糖衣片，除去包衣显棕黄色;味极苦。
【适应症/功能主治】舒肝健脾。用于急、慢性肝炎属肝郁脾虚证。
【规格型号】0.2g*60s
【用法用量】口服，糖衣片一次4片，一日3次。宜在饭后30分钟服用。
【不良反应】尚不明确。
【禁忌】尚不明确。
【注意事项】尚不明确。
【药物相互作用】如与其他药物同时使用可能会发生药物相互作用，详情请咨询医师或药师。
【贮藏】密封。
【包装】0.2g*60s/盒。
【有效期】24月
【批准文号】国药准字Z6449
【生产企业】江苏正大清江制药有限公司
篇3：肝康颗粒说明书
1 实验材料
1.1 仪器
DHP-9082电热恒温培养箱;SPX-150B-Z生化培养箱;TMQ-R灭菌器;净化工作台VS-1300L-U。
1.2 药品与试剂
肝康灵颗粒(规格:7 g/袋，批号:121224、121225、121226，南昌市第九医院制剂室);靛基质。
1.3 菌种
大肠埃希菌(Escherichia coli,coli)[CMCC(B)44102]、金黄色葡萄球菌(Staphyloccocus aureus)[CMCC(B)26003]、枯草芽孢杆菌Bacillus subtilis[CMCC(B)63501]、白色念珠菌Monilia albican[CMCC(F)98001]、黑曲霉[CMCC(F)98003]。
1.4 培养基
营养琼脂培养基、营养肉汤培养基、玫瑰红钠胖伴有睡眠呼吸暂停综合征以及其他有循环系统合并症的患者用药应谨慎，要调整好药物剂量与浓度，严密监测，以确保患者安全。琼脂培养基、改良马丁培养基、改良马丁琼脂培养基、胆盐乳糖培养基、4-甲基伞形酮葡萄苷酸培养基(MUG)。菌种和培养基均购于江西省食品药品检定所。
1.5 稀释剂
p H7.0无菌氯化钠-蛋白胨缓冲液，0.9%无菌氯化钠溶液。
2 实验方法
2.1 菌液制备
接种大肠埃希菌、金黄色葡萄球菌、枯草芽孢杆菌的新鲜培养物至10 ml营养肉汤培养基中，35℃培养24 h，用0.9%无菌氯化钠溶液制成每1 ml含菌数为50～100cfu的菌悬液，接种白色念珠菌的新鲜培养物至10 ml改良马丁培养基，25℃培养48 h，用0.9%无菌氯化钠溶液制成每1ml含菌数为50～100 cfu的菌悬液，接种黑曲霉菌的新鲜培养物至改良马丁琼脂斜面培养基中，25℃细菌培养7 d，加入4 ml 0.9%无菌氯化钠溶液[2]，将霉菌孢子洗脱，然后吸出孢子悬液(用管口带有薄的无菌棉花或纱布能过滤菌丝的无菌毛细吸管)至无菌试管内，用0.9%无菌氯化钠溶液制成每1ml含孢子数为50～100 cfu的孢子悬液。
2.2 供试液制备
取供试品10 g，加入p H7.0无菌氯化钠-蛋白胨缓冲液至100 ml，振摇，使成1∶10的供试液。
2.3 肝康灵颗粒微生物限度检查回收率测定
菌液组:分别取5种菌液(50～100 cfu/ml)各1 ml，注入平皿，加入相应培养基，按菌落计数方法测定所加的试验菌数。供试品对照组:取供试液(1∶10)1 ml，注入平皿，加入相应培养基，培养，计数。实验组:取供试液(1∶10)1 ml和含菌悬液(50～100 cfu/ml)1 ml至平皿后，分别注入相应的培养基，细菌注入营养琼脂培养基，霉菌和酵母菌注入玫瑰红钠琼脂培养基，细菌在33℃培养48 h，霉菌和酵母菌在27℃培养72 h，观察结果[3]，点计菌落数。
稀释剂对照组:取稀释剂(p H7.0无菌氯化钠-蛋白胨缓冲液)1 ml，加入1 ml菌液(50～100cfu/ml)，注入培养基。
每株试验菌平行制备2个平皿。做3次独立的平行试验，分别计算各试验菌每次试验的回收率，采用平皿计数法。结果见表1。
2.4 控制菌检查方法的验证
实验组:取3个批次的供试液(1∶10)10 ml及大肠埃希菌液(10～100 cfu/ml)1 ml，加入胆盐乳糖培养基至100 ml;取3个批次的供试液(1∶10)10ml，加入大肠埃希菌液1 ml(10～100 cfu/ml)作为阳性对照;另取稀释剂10 ml加入胆盐乳糖培养基至100 ml作为阴性对照。阴性菌对照组:取3个批次的供试液(1∶10)10 ml，加入金黄色葡萄球菌液(10～100 cfu/ml)1 ml。35℃培养24h，观察结果。取实验组增菌液0.2 ml，接种至含5 ml MUG培养基的试管中，培养，于5 h、24 h在366 nm紫外线下观察，然后沿试管壁滴加靛基质，液面呈玫瑰红色环为靛基质阳性，呈试剂本色，为靛基质阴性。
3 结果
3.1 验证结果
按照常规法，3个批次的供试品大肠埃希菌检查，实验组均可检出试验菌，阴性组和阴性菌对照组均无生长。
3.2 回收率测定结果
由表1可知，该供试品对大肠埃希菌、金黄色葡萄球菌、枯草芽孢杆菌、白色念珠菌、黑曲霉菌的回收率均高于70%，稀释剂对5种实验菌的回收率均高于70%，控制菌检查阳性菌生长良好，阴性菌未检出。
4 讨论
微生物限度检查法是检查非最终灭菌制剂及原辅料受微生物污染程度的方法。检查项目包括细菌、霉菌、酵母菌及控制菌检查[4]。本制剂属于口服制剂，按照微生物限度检查法中常规法检查，该供试品对大肠埃希菌、金黄色葡萄球菌、枯草芽孢杆菌、白色念珠菌、黑曲霉菌的回收率均高于70%，稀释剂对5种实验菌的回收率均高于70%，故本品无抑菌作用，控制菌检查选择大肠埃希菌作为试验用菌株，金黄色葡萄球菌作为阴性菌对照菌株，且阳性菌生长良好，说明本品对大肠埃希菌没有抑菌作用，阴性菌未检出，说明该控制菌检查方法专属性好，可用于控制菌检查。
通过本实验得知，在制剂处方、生产工艺及监测环境不变的情况下，采用常规法可以进行本品的微生物限度检查。
摘要：目的 建立肝康灵颗粒微生物限度检查方法,并对方法进行验证。方法 按照中国药典2010版一部方法对3个批号的肝康灵颗粒进行微生物限度检查方法验证,采用平皿记数法,接种5种实验菌验证,分别计算各实验菌的回收率。结果 各实验菌的回收率均>70%。大肠埃希菌可采用常规法检出。结论 采用常规法可以进行肝康灵颗粒微生物限度检查。
关键词：肝康灵颗粒,微生物限度检查,验证,常规法
参考文献
[1]苏德模,马绪荣.药品微生物学检验手册.北京:华龄出版社,2007:209-234.
[2]宋勤,杜平华.中成药微生物限度检查方法的探讨.中国药事,2006,20(1):46-48.
[3]包东升.小儿咳喘颗粒微生物限度检查方法的验证.海峡药学,2010,22(8):94-95.
[4]国家药典委员会.中国药典(一部).北京:中国医药科技出版社,2010:附录79-85.
篇4：溃疡颗粒说明书
【商品名称】溃疡颗粒
【拼音全码】KuiYangKeLi
【主要成份】甘草浸膏、海螵蛸、白及、黄芩、延胡索(醋炙)、薏苡仁(麸炒)、泽泻、天仙子。
【性状】溃疡颗粒为颗粒剂。
【适应症/功能主治】健胃，消炎，止痛。用于胃溃疡，十二指肠溃疡，急慢性胃炎。
【规格型号】10g*10袋
【用法用量】开水冲服，1袋(10g)，一日3次。
【不良反应】尚不明确。
【禁忌】心脏病、心动过速、青光眼患者及孕妇忌服。
【注意事项】高血压、肾炎、水肿患者慎服。
【药物相互作用】如与其他药物同时使用可能会发生药物相互作用，详情请咨询医师或药师。
【贮藏】密封。
【包装】每盒10袋。
【有效期】36月
【执行标准】卫生部药品标准中药成方制剂第十册
【批准文号】国药准字Z11020965
【生产企业】北京同仁堂科技发展股份有限公司制药厂
篇5：补白颗粒说明书
【商品名称】补白颗粒(南洋)
【拼音全码】BuBaiKeLi(NanYang)
【主要成份】补骨脂、白扁豆、淫羊藿、黑大豆、赤小豆、丹参、柴胡、苦参。
【性状】补白颗粒(南洋)为棕黄色的颗粒;味甜、微苦。
【适应症/功能主治】健脾温肾。用于慢性白细胞减少症属脾肾不足者。
【规格型号】15g*9袋
【用法用量】开水冲服，一次15g，一日3次。
【不良反应】见说明书
【禁忌】尚不明确。
【注意事项】见说明书
【药物相互作用】如与其他药物同时使用可能会发生药物相互作用，详情请咨询医师或药师。
【贮藏】密封。
【包装】15g*9袋/盒。
【有效期】24月
【批准文号】国药准字Z6047
【生产企业】浙江南洋药业有限公司
篇6：黄芪颗粒说明书
【商品名称】黄芪颗粒
【拼音全码】HuangQiKeLi(HanFang)
【主要成份】黄芪。
【性状】黄芪颗粒为淡黄色的颗粒;味甜。
【适应症/功能主治】补气固表，利尿，托毒排脓，生肌。用于气短心悸，虚脱，自汗，体虚浮肿，慢性肾炎，久泻，脱肛，子宫脱垂，疮口久不愈合。
【规格型号】15g*10袋
【用法用量】开水冲服，每次15克，一日2次。
【不良反应】尚不明确。
【禁忌】糖尿病患者禁服。
【注意事项】1.忌辛辣、生冷、油腻食物。2.感冒发热病人不宜服用。3.黄芪颗粒宜饭前服用。4.高血压、心脏病、肝病、肾病等慢性病患者应在医师指导下服用。5.服药2周症状无缓解，应去医院就诊。6.儿童、孕妇应在医师指导下服用。7.对黄芪颗粒过敏者禁用，过敏体质者慎用。8.黄芪颗粒性状发生改变时禁止使用。9.儿童必须在成人监护下使用。10.请将黄芪颗粒放在儿童不能接触的地方。11.如正在使用其他药品，使用黄芪颗粒前请咨询医师或药师。
【药物相互作用】如与其他药物同时使用可能会发生药物相互作用，详情请咨询医师或药师。
【贮藏】密封。
【包装】铝塑复合热合包装，10袋/盒。
【有效期】24月
【执行标准】wS3-B-2224-96
【批准文号】国药准字Z3254
【生产企业】贵州汉方药业有限公司
黄芪颗粒(汉方)的功效与作用黄芪颗粒(汉方)补气固表，利尿，托毒排脓，生肌。用于气短心悸，虚脱，自汗，体虚浮肿，慢性肾炎，久泻，脱肛，子宫脱垂， 疮口久不愈合。
黄芪颗粒服用常见问题
黄芪颗粒是临床上常用的药物，适用一些体质虚弱的患者服用。黄芪颗粒是纯天然的药物，对人体疾病无害，深受患者欢迎。当人们觉得一个药好的时候，就会想长期服用。那么，黄芪颗粒可以长期服用吗?
黄芪颗粒是可以长期服用的，但也不能过量的服用。黄芪颗粒的服用方法是开水冲服，一次4g(1袋)，一日2次，宜饭前服用。建议患者连续服用黄芪颗粒2个月以上。服用过程中应忌辛辣、生冷、油腻食物。感冒发热病人不宜服用。服药2周症状无缓解，应去医院就诊。黄芪颗粒性状发生改变时禁止服用。如正在服用其他药品，使用黄芪颗粒前请咨询医师或药师。
黄芪颗粒的作用是补气固表，利尿，托毒排脓，生肌。用于气短心悸，虚脱，自汗，体虚浮肿，慢性肾炎，久泻，脱肛，子宫脱垂，痈疽难溃，疮口久不愈合。为淡黄色的颗粒;味甜。
黄芪颗粒的成份是黄芪，在中医角度来说，黄芪，性甘温，归肺经，有补气升阳、益卫固表之功能。现代医学研究表明，黄芪含皂甙、蔗糖、多糖、多种氨基酸、叶酸及硒、锌、铜等多种微量元素。黄芪有增强机体免疫功能、保肝、利尿、抗衰老、抗应激、降压和较广泛的抗菌作用。黄芪不仅能扩张冠状动脉，改善心肌供血，提高免疫功能，而且能够延缓细胞衰老的进程。
篇7：肝康颗粒说明书
Recently,chromatographic fingerprint technique,as a more meaningful formulation for controlling the quality of TCM,has emphasized on the systemic characterization of compositions of samples and focus on identifying the stability of the plants.Fingerprint technique has been introduced and accepted by WHO as a strategy for the assessment of herbal medicines[7].Because of its advantages and popularization,TLC and HPLC fingerprint analysis have been received as the first choice[8,9,10].
Up to now,most of analytical methods established for the quality control of the crude drug were involved in the qualitation or quantification of one or two of components from only one comprising herb[11,12].However,the biological activities of these single chemical compounds alone could not fully account for the potency and efficacy of parent TCM complex.It is possible that the therapeutic effects of TCM complex are ultimately the results of a concerted action of multiple chemicals on the corresponding cellular targets.Considering all these factors discussed above,we made simultaneous determination of two bioactive components from two different raw drugs by HPLC-UV,using bioactive Emodin[13]and Icariin[14]as marker compounds.Also,three kinds of raw drugs were identified by TLC with Psoralen[15],Astragaloside[16]and Berberine[17]being marker compounds,respectively.In this paper,the structures of these marker compounds were shown in Figure 1.
1 Experimental
1.1 Apparatus
ALC-10ATVPhigh-performanceliquid chromatography system including a VP-ODS(150×4.6 mm)chromatographic column and UV-2450spectrophotometer(Shimadzu,Japan)was used to acquire chromatograms.Ultrasonic extraction device(Kedao ultrasound Instrument Co.Ltd.,Shanghai,China)was used for sample extraction.
1.2 Materials
GKG was the gift given by Hunan Yuanhang Pharmaceutical Co.Ltd.(Batch 051001,051002,051101).All crude drugs were purchased from the city of Changsha,China,and identified by Dr.Tang Yijia at Hunan Provincial Institute for Drug Control.The five reference substances of Emodin(Lot 110756-200110),Icariin(Lot110737-200312),Psoralen(Lot110739-200512),Astragaloside(Lot 110781-200512)and Berberine(Lot 110713-200208)were purchased from the National Institute for the Control of Pharmaceutical and Biological Products,China.HPLC grade methanol and acetonitrile,from Tedia company(U.S.A),were used for preparation of mobile phase.Other reagents were of analytical grade.
1.3 Qualitative identification
1.3.1 Reference and sample solution preparation
Preparation of reference solution:Standard solutions of three medical materials were prepared respectively in ethanol at concentration of 1.500 mg/m L for Psoralen,0.500 mg/m L for Astragaloside and Berberine each.
Preparation of sample solution:For Ficus simplicissima Lour.root and Astragalus monghbolicus(Bge.)Hsiao,15.0 g of GKG(accurately weighed)were dissolved respectively in 100 m L of methanol for ultrasonic extraction for 20 min,filtered.Then the filtrate was evaporated to dryness in water bath,dissolved in 8 m L of water and flowed through D101macroporous resin column(2.5 cm of diameter,30 cm of height).After that,400 m L of water,40%ethanol and60%ethanol were used one after another to elute.At last,60%ethanol solution was collected,evaporated,dissolved in 2 m L of methanol for use.For Mahonia bealei(Fort)Carr,instead of 8 m L of water to dissolve,20 m L of 0.5 mol/L hydrochloric acid solution were used,then extracted twice with 40 m L of ethyl acetate each,abandoned ethyl acetate liquid,regulated with ammonia to make p H=(12±0.05).After that,30 m L of chloroform were used to extract twice,then evaporated the combined chloroform liquid.Finally,2 m L of methanol were utilized to dissolve the residue as a sample solution for the test.
Preparation of the positive control solution of medicinal herbs:According to the above-mentioned method,Ficus simplicissima Lour.root(2 g),Astragalus monghbolicus(Bge.)Hsiao(2 g)and Mahonia bealei(Fort)Carr(3 g)were respectively made to be the positive control solution.
Preparation of negative control solution:It contains7 herbs lack of Ficus simplicissima Lour.root or Astragalus monghbolicus(Bge.)Hsiao or Mahonia bealei(Fort)Carr.
1.3.2 Chromatography of TLC
According to TLC test(see appendix VIB,Chinese Pharmacopoeia,2005),Ficus simplicissima Lour.,Astragalus monghbolicus(Bge.)Hsiao and Mahonia bealei(Fort)Carr were identified in their optimal reagent systems.20μL of sample solution,20μL of negative control solution,4μL of reference solution and 4μL of positive control solution were applied onto the same silicon G thin-layer plate.The plate was dried in a current of air and developed with a mobile phase of n-hexane-ethyl acetate(4∶1,v/v)for Ficus simplicissima Lour.,chloroform-ethyl acetate-methanol-water(20∶40∶22∶10,v/v/v/v)for Astragalus monghbolicus(Bge.)Hsiao and benzene-ethyl acetate-isopropyl alcohol-methanol-concentrated ammonia(6∶3∶1.5∶1.5∶0.5,v/v/v/v/v)for Mahonia bealei(Fort)Carr under laboratory condition[temperature(25±3)℃].All spots were visualized in UV detection at 254 nm for Ficus simplicissima Lour.and 365 nm for Mahonia bealei(Fort)Carr.As for Astragalus monghbolicus(Bge.)Hsiao,the developed plate was immersed in freshly prepared sulphuric acid alcohol solution,and the resultant plate was then heated at 105℃for 5 min until the spots were clear to see.
1.4 Quantitative determination
1.4.1 Referenceandsample
solution preparation 1.20 mg Emodin reference substance and2.00 mg Icariin reference substance were transferred separately into 10 m L measuring flasks and mixed with methanol.The content of each flask was completed to volume with the mobile phase to get the concentrations of 0.120 mg/m L of Emodin or 0.200 mg/m L of Icariin,then filtered through 0.45μm filters.
For the Emodin,2.0 g of GKG were used to prepare the sample solution.It was dissolved in 25mL methanol,extracted three times with chloroform(30,20 and 15m L)and dried,then the residue was dissolved in 10mL of methanol,filtered by 0.45μm filter.As for the Icariin,4.0g of GKG were dissolved in 50 m L of methanol,filtrated and dried.The residue was dissolved in 25 m L of methanol,filtrated with 0.45μm filter and used for HPLC analysis.
We also prepared negative control solution which contains 7 herbs lack of Rumex japonicus Houtt root or Epimedium brevicornum Maxim.
1.4.2 Chromatographic conditions of HPLC
The samples were then chromatographed under the following chromatographic conditions:Chromatographic column:VP-ODS 150 mm×4.6 mm analytical column(Shimadzu).Mobile phase:methanol-0.25%phosphoric acid(80∶20,v/v)for Emodin,acetonitrile-water(26∶74,v/v)for Icariin.The final p H-value was adjusted to(3.0±0.07)with o-phosphoric acid by a p H-meter.Flow rate:1.1 m L/min for Emodin and 1.0m L/min for Icariin.Column temperature:45℃for Emodin and 30℃for Icariin,with UV detection at 436nm for Emodin and 270 nm for Icariin.
1.4.3 Analytical data treatment
Reference solution,sample solution and negative sample solution were injected precisely into liquid chromatography for determination.The relative peak area ratios were then plotted versus the corresponding concentrations of Emodin or Icariin to get the calibration graph and compute the corresponding regression equation.Then concentrations of Emodin and Icariin were calculated from the linear regressions.
2 Results and discussion
2.1 Identification by TLC
The sample tracks were scanned at UV light.It was clearly evident that no interfering compound eluted in the sample tracks to affect the quantitation of the targeted marker.As the results were showed in Figure 2,the spots of the sample solution showed significantly the same as the reference substance,the negative samples in the corresponding location displayed no interference.
To identify the herbs,the chief active components or index ingredients should be choosed,such as Ficus simplicissima Lour.Root,Astragalus monghbolicus(Bge.)Hsiao and Mahonia bealei(Fort)Carr in our study.For Ficus simplicissima Lour.,GKG was originally resolved in methanol for ultrasonic extraction and filtered through 0.45μm membrane.Then the filtrate was extracted by ethyl acetate three times,condensed and spotted the plate,using N-hexane-ethyl acetate as developing agent.The results showed that there appeared orange spot rather than blue white in the corresponding place of reference substance,it was evident that there was interference.Therefore,macroporous adsorptive resins were used for purification,and the spots were clear to see.For Astragalus monghbolicus(Bge.)Hsiao and Mahonia bealei(Fort)Carr,official methods in Chinese Pharmacopiea were used and refined.The suitable amount of spotting for Astragalus monghbolicus(Bge.)Hsiao was 25～30μL.
2.2 Assaying by HPLC
The results showed that the peak of Emodin or I-cariin in the sample was well-resolved peak,and the resolution with its adjacent chromatographic peaks was more than 1.5.The calculated theoretical plate number was more than 3,000 according to the peak of Emodin or Icariin.At the same time,the negative chromatography lacks of a corresponding peak in the corresponding position of the peak of Emodin or Icariin,which explained that there was no negative interference.See Figure 3 and Figure 4.
2.3 Method validation for HPLC
Validation of quantitative method includes evaluation of the following performance parameters,such as specificity,reproducibility,linearity,limits of sensitivity,precision,stability,recovery and robustness,according to the guidelines of ICH[18]and International Union of Pure and Applied Chemistry(IUPAC)[19].
2.3.1 Specificity and reproducibility
10μL of reference solution,10μL of sample solution and 10μL of negative sample solution were injected precisely into liquid chromatography for determination under the optimum condition mentioned above.The sample solution has a corresponding peak in the corresponding position of the peak of reference solution with the same retention time,7.5 min for Emodin and 22 min for Icariin respectively.Moreover,there was no negative interference.See Figure 3 and Figure 4.
For intraday and inter-day reproducibility test,six portions of sample solution for Emodin or Icariin were each analyzed to determine the intraday and inter-day reproducibility of the peak areas under the optimum conditions in this experiment.R.S.D.of the peak areas was both quite low(Table 1).
2.3.2 Linearity and detection limit
A stock solution of 0.12 mg/m L of Emodin or 0.20 mg/m L of Icariin was prepared in a 50 m L volumetric flask by dissolving 6 mg of Emodin or 10 mg of Icariin in mobile phase.Appropriate amounts of the stock solution were injected to obtain solutions containing 120.0,480.0,960.0,1 440.0,1920.0 and 2 400.0 ng of Emodin respectively and 200.0,800.0,1 600.0,2 400.0,3 200.0 and 4 000.0 ng of I-cariin respectively.Each solution was injection in triplicate into the chromatograph.The series of the standard solution of Emodin or Icariin were tested to determine the linearity between the standard concentrations and the peak areas.The calibration curve was prepared with the absolute amount(ng)as independent variable(X)and the peak area of Emodin or Icariin as dependent variable(Y).The corresponding regression equations were computed and found to be:Y=2 375.1x+75 229(r=0.9996)for Emodin and Y=2 105.2x+46 846(r=0.9994)for Icariin.
Serial amounts of Emodin or Icariin in mobile phase were performed.A linear relationship was obtained in the range of 120～2 400 ng for Emodin or200～4 000 ng for Icariin.
2.3.3 Precision and stability
Repeatability was calculated by analyzing 6 samples.The precisions expressed as the relative standard deviation(R.S.D.)for peak area were determined for Emodin or Icariin standards by repeated analysis.The precision results obtained from Table 1 showed that the R.S.D.for peak area was both quite low.
For stability test,the sample solution(ethanol extract)was analyzed every 2 h within 10 h(n=6).R.S.D.=2.57%for Emodin and R.S.D.=3.18%for Icariin(n=6).
2.3.4 Sample analysis,recovery and robustness
The contents of the Emodin or Icariin were calculated from the linear regression.The average contents in three lots of GKG are 0.869 mg/g(CV=2.3%)for Emodin and1.014 mg/g(CV=3.1%)for Icariin respectively.According to 80%average value of the total number,the value is 0.695 mg/g for Emodin and 0.811 mg/g for Icariin respectively.Considering the source of medicinal herbs and the actual process of production and storage,we set a limit that at least 0.60 mg/g of Emodin and 0.80 mg/g of Icariin should be contained in the finished drug.
Note:R.S.D.Relative standard deviation;Data are means±R.S.D.of six replicates
The recovery experiment was performed for six times by adding Emodin or Icariin to the sample solution according to the procedure described above.The amounts of Emodin or Icariin recovered in relation to the results obtained in the intermediate precision study were calculated.The mean recoveries were 98.75%for E-modin and 98.83%for Icariin(Table 1).
Robustness was examined by changing slightly in the chromatography conditions,such as the proportion of mobile phase,flow rate and column temperature.In all the deliberately varied chromatographic conditions,the chromatogram of sample solution showed satisfactory resolution(Table 2).
Note：覮All the values of R.S.D.<5%
3 Conclusions
TLC is a glob ally accepted rational and practical solution to characterize the crude plant drug,pharmacologically active constituent enriched standardized extracts and their formulations.This standardized TLC procedure may be used effectively for screening the Ficus simplicissima Lour.root,Astragalus monghbolicus(Bge.)Hsiao and Mahonia bealei(Fort)Carr.as well as quality evaluation of the plant.