苗药组方二岩虎果无糖颗粒质量标准研究及药效评价  

Quality Standard and Efficacy Evaluation of Miao Drug Prescription Eryanhuguo Sugar-Free Granules

作　　者：饶海 刘永琴 罗忠圣 梁芳瑜 徐昌艳[2] 覃容贵[2] RAO Hai;LIU Yongqin;LUO Zhongsheng;LIANG Fangyu;XU Changyan;QIN Ronggui(Guiyang Yunyan District People's Hospital,Guiyang,Guizhou,China 550001;Guizhou Medical University,Guiyang,Guizhou,China 550025;Guizhou Key Laboratory of Natural Product Chemistry of Chinese Academy of Sciences,Guizhou Medical University,Guiyang,Guizhou,China 550014;State Key Laboratory for the Effectiveness and Utilization of Medicinal Plants,Guiyang,Guizhou,China 550025)

机构地区：[1]贵州省贵阳市云岩区人民医院,贵州贵阳550001 [2]贵州医科大学,贵州贵阳550025 [3]贵州医科大学天然产物化学重点实验室,贵州贵阳550014 [4]省部共建药用植物功效与利用国家重点实验室,贵州贵阳550025

出　　处：《中国药业》2022年第5期71-75,共5页China Pharmaceuticals

基　　金：贵州省中药现代化科技产业研究开发专项项目[黔科合SY字〔2014〕3008-5]。

摘　　要：目的建立苗药组方二岩虎果无糖颗粒的质量标准,并评价其药效。方法采用薄层色谱法对二岩虎果制剂中岩豇豆、岩白菜、虎杖进行定性鉴别;按2020年版《中国药典(四部)》颗粒剂项下要求,对制剂的粒度、水分、溶化性、干燥失重、重金属和砷盐进行检查;采用高效液相色谱法测定制剂中石吊兰素含量,色谱柱为Dikma-C_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(68∶32,V/V),流速为1 mL/min,检测波长为334 nm,柱温为30℃,进样量为20μL。将80只SPF级KM种小鼠随机分为空白对照组(生理盐水)、传统汤剂组(1 g/mL)、颗粒剂组(0.387 g/mL)、阳性对照组(复方岩白菜素2.8 mg/mL或阿司匹林10 mg/mL),各10只,平行2组。各组小鼠均连续给药7 d,分别于末次给药1 h后用氨水致小鼠咳嗽,或于小鼠右耳两面涂抹二甲苯致炎,分别统计各组小鼠的咳嗽潜伏期、3 min内咳嗽次数,并计算肿胀抑制率。结果岩豇豆、岩白菜、虎杖药材的薄层色谱斑点均显色清晰,专属性强,分离度好,且阴性对照无干扰;3批样品不能通过1号筛与能通过5号筛颗粒粒度的总和低小于15%,水分均低于8%,全部在5 min内溶解,减失质量均不超过2.0%,重金属含量均小于1×10^(-5),砷盐含量均小于2×10^(-6)。石吊兰素质量浓度在5~50μg/mL范围内与峰面积线性关系良好,r=0.9996(n=5);含量测定精密度、稳定性、重复性试验的RSD均小于2.0%(n=6),平均加样回收率为102.32%,RSD为3.70%(n=6)。与传统汤剂组比较,颗粒剂组小鼠的咳嗽潜伏期延长,3 min咳嗽次数减少,肿胀抑制率降低,但差异均不显著(P>0.05)。结论所建立的方法操作简便,结果准确,稳定性和重复性均较好,可用于二岩虎果无糖颗粒的质量控制,且颗粒剂药效良好。Objective To establish the quality standard of Miao drug prescription Eryanhuguo Sugar-Free Granules and to evaluate its efficacy.Methods Lysionotus Herba,Bergenia Rhizoma and Polygonum Cuspidatum Rhizoma et Radix in the Eryanhuguo preparation were qualitatively identified by the thin-layer chromatography(TLC)method.The particle size,moisture,solubility,loss on drying,heavy metals and arsenic salt of the preparation were checked according to the requirements of granules in the Chinese Pharmacopoeia(2020 Edition,VolumeⅣ).The content of clenbuterol in the preparation was determined by the high-performance liquid chromatography(HPLC)method,the chromatographic column was Dikma-C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was methanol-water(68∶32,V/V),the flow rate was 1 mL/min,the detection wavelength was 334 nm,the column temperature was 30℃,and the injection volume was 20μL.A total of 80 SPF KM mice were randomly divided into the blank control group(normal saline),traditional decoction group(1 g/mL),granule group(0.387 g/mL)and positive control group(2.8 mg/mL of compound bergenin or 10 mg/mL of aspirin),with 10 mice in each group,and then the two groups were parallelled.Mice in each group were given drugs continuously for 7 d.One hour after the last administration,the mice coughed with ammonia or were inflamed with xylene on both sides of the right ear.The cough latency and the times of coughs within 3 min were counted,and the swelling inhibition rate was calculated.Results The TLC spots of Lysionotus Herba,Bergenia Rhizoma and Polygonum Cuspidatum Rhizoma et Radix showed clear color,had strong specificity and good separation,and the negative samples had no interference.The total particle size of the three batches of samples that could not pass the No.1 sieve and that could pass the No.5 sieve was less than 15%,the water content was less than 8%,all of them were dissolved within 5 min,the loss mass was not more than 2.0%,the content of heavy metals was less than 1×10^(-5),and the content of arsenic

关 键 词：二岩虎果无糖颗粒 薄层色谱法 高效液相色谱法 药效 石吊兰素 质量标准 小鼠 

分 类 号：R932[医药卫生—生药学] R286.0[医药卫生—药学]