CN106980000A - 灯盏花定性定量中药饮片的质量标准与制造工艺 - Google Patents
灯盏花定性定量中药饮片的质量标准与制造工艺 Download PDFInfo
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Abstract
本发明提供了一种安全、高效、便捷的灯盏花中药饮片。本发明提供的灯盏花定性定量中药饮片制造工艺,采用一种炮制工艺将符合质量标准的灯盏花制备成中药饮片,可冲泡服用改变传统煎煮服用方法,同时提供一种灯盏花饮片质量标准,在现有质量标准的基础上增加相关检测项目,并提高含量测定中的野黄芩苷总量的标准限度,可有效对灯盏花饮片的质量进行控制,提高了药品的质量标准,增加了用药安全性。
Description
技术领域
本发明涉及中药领域,具体为灯盏花定性定量中药饮片的质量标准、操作规程与制造工艺。
背景技术
灯盏花(Gerbera jamesonii),是菊科植物短葶飞蓬Erigeron breviscapus(Vant.)Hand-Mazz的干燥全草,又名灯盏细辛、东菊,主要分布于我国西南地区,尤以云南较多。夏、秋二季采挖,除去杂质,晒干。首载于《滇南本草》,《中国药典》1977年版一部曾予收载。灯盏花性寒、微苦、甘温辛,具有微寒解毒、祛风除湿、活血化瘀、通经活络、消炎止痛的功效。过去30多年来,我国学者从该植物分离出了黄酮、咖啡酰奎尼酸、γ-吡喃酮、香豆素、木脂素、萜类、甾醇、芳香酸、脂肪酸及其他类型化合物,其中的酚酸类成分,特别是黄酮和咖啡酰奎尼酸类被普遍认为是灯盏花的抗氧化和心脑血管活性成分。为进一步阐明灯盏花的化学成分,对灯盏花的乙醇提取物进行了分离,得到十二个化合物,分别鉴定为槲皮素-3-O-β-D-葡萄糖苷、5,7-二羟基色原酮、3-O-咖啡酰-γ-奎尼内酯、柚皮素、3,5-二-O-咖啡酰奎尼酸、3,4-二-O-咖啡酰奎尼酸、4,5-二-O-咖啡酰奎尼酸、1,3-二-O-咖啡酰奎尼酸、1,5-二-O-咖啡酰奎尼酸、3-O-咖啡酰奎尼酸、4-O-咖啡酰奎尼酸和绿原酸。目前灯盏花注射液在临床上除主要用于心脑血管系统疾病外,在糖尿病、肾病、颈性眩晕、老年性疾病的治疗上也有较好的疗效。灯盏花作为常用中药,具有强大的开发潜力。随着社会对灯盏花的需求量日益增加,传统煎煮服用较为耗时费力,因此迫切需要一种可冲泡服用的灯盏花中药饮片。
本发明所要解决的问题是解决目前市场上的普遍存在中药饮片疗效不明显与中药材因环境污染而重金属超标、农药残留超标等质量问题。
中药饮片是中国中药产业不可缺失的部分,是中医临床辩证施治必需的传统武器,其品质直接影响中医临床防病、治病的疗效,另外针对现代人快速的生活节奏,本发明提供的高品质、可冲泡服用改变传统煎煮服用方法的中药饮片有较大的市场需求。
附图说明
附图1是灯盏花定性定量中药饮片生产工艺流程图。
发明内容
为了解决上述问题,本发明提供的灯盏花定性定量中药饮片的质量标准与制造工艺,增加对药屑杂质、重金属及有害元素、有机氯农药残留量、黄曲霉毒素B1、二氧化硫残留量的检测,并将含量测定中的野黄芩苷总量的标准限度从0.30%提高至0.33%。并通过特定的工序生产出灯盏花中药饮片,确保中药饮片符合高标准高品质的要求。
本发明提供的灯盏花定性定量中药饮片的制造工艺,包括以下步骤:
A10、净制:清除混在药物中的杂质及霉变品等,或将药物按大小进行分档,以便达到洁净或进一步加工处理。
A20、润药:净制后的药材放入洗润池中,喷水堆润6-8h,至药材彻底润透。
A30、切制:按全自动高速切片机操作规程操作,调好刀距0.4mm,进行切药。
A40、干燥:采用热风循环烘箱进行干燥,将药材铺于烘箱架子上,摊铺厚度均匀,厚度在3cm以下。打开开关,开启加热开关、风机,在温度60±2℃进行干燥,在温度达到设定温度后干燥5-7h,干燥完毕,关闭加热开关,继续吹风,待箱内温度降下至35~40℃,关闭风机。干燥后岗位人员需填写中间产品请检单,交质量部由QA取样进行水分检查。
A50、包装:根据本品包装规格要求进行包装。包装前需对包装间进行检查,确认包装生产线的清场已经完成,并核对包装材料是否符合要求。内包装:在设备上调整好需要印制的生产日期、批号,QA监控,称取规定重量的药材放入料斗中,用封口机封口,要求做到封口严密、平整、美观外包装:在设备上调整好需印制的生产日期及批号,QA监控,在外包装盒子上打印批号、生产日期,打印过程中需注意批号及生产日期是否清晰。将内包装完成后的饮片及检验报告书放入外包盒中,4袋/盒。将每10盒饮片,套入1个热缩膜中,进行热收缩;热收缩后装入大纸箱中,240盒/箱。操作过程中,QA随时抽检。
A60、成品:包装后岗位人员需填写成品请检单,交质量部由QA取样进行产品检查。
增加对药屑杂质、重金属及有害元素、有机氯农药残留量、黄曲霉毒素B1、二氧化硫残留量的检测,并将含量测定中的野黄芩苷总量的标准限度从0.30%提高至0.33%。修订后的灯盏花定性定量中药饮片的质量标准如下所示:
灯盏花饮片
拼音名称:Dengzhanhua Yinpian
包装:纯铝复合膜包装。
【性状】取本品适量,在日光下观察,本品呈不规则碎,质脆,断面黄白色,有髓或中空。叶皱缩、破碎,黄绿色。嗅之,气微香,尝之,味微苦。
【鉴别】
显微鉴别
仪器及用具:中药粉碎机、药典筛、显微镜、酒精灯
试剂及试液:水合氯醛试液、甘油醋酸试液、甘油乙醇试液、稀甘油(试剂均使用分析纯,实验用水为纯化水)
测定:取本品叶适量,切片置载玻片上,滴加甘油醋酸试液、水合氯醛试液或其他试液1~2滴,盖上盖玻片。必要时滴加水合氯醛试液后,在酒精灯上加热透化,并滴加甘油乙醇试液或稀甘油,盖上盖玻片,于显微镜下观察:本品叶表面观:表皮细胞壁波状弯曲,有角质线纹,气孔不定式。非腺毛1~8细胞,长约180~560μm。腺毛头部1~4细胞,柄1至多细胞。
结果判定:本品叶表面观:表皮细胞壁波状弯曲,有角质线纹,气孔不定式。非腺毛1~8细胞,长约180~560μm。腺毛头部1~4细胞,柄1至多细胞。
高效液相色谱鉴别
仪器及用具:中药粉碎机、分析天平、药典筛、超声波清洗机、高效液相色谱仪
试剂及试液:甲醇、磷酸、三氯甲烷(其中甲醇为色谱纯,其他试剂为分析纯,实验用水为纯化水)
测定及结果判定 取本品,照(含量测定)项下的方法试验,供试品色谱应呈现与对照品色谱保留时间相一致的色谱峰。
【检查】
检查
药屑、杂质
仪器及用具:中药粉碎机、分析天平、药典筛
照杂质检查法(通则2301)测定。取供试品约100g(精确到0.1g),摊开,拣出杂质,用6号筛筛出药屑,合并,称重,计算其在供试品中的量(%)。
结果判定:本品药屑、杂质不得过3%。
水分
仪器及用具:中药粉碎机、分析天平、药典筛、电热恒温鼓风干燥箱、称量瓶
测定及结果判定:照水分测定法(通则0832第二法)测定。取供试品2~5g,平铺于干燥至恒重的扁形称量瓶中,厚度不超过5mm,疏松供试品不超过10mm,精密称定,开启瓶盖在100~105℃干燥5小时,将瓶盖盖好,移置干燥器中,放冷30分钟,精密称定,再在上述温度干燥1小时,放冷,称重,至连续两次称重的差异不超过5mg为止。根据减失的重量,计算供试品中含水量(%)。
结果判定:本品水分不得过12.0%。
总灰分
仪器及用具:中药粉碎机、分析天平、药典筛、马弗炉、电炉、坩埚
测定及结果判定:照灰分测定法(通则2302)测定。取供试品2~3g(如须测定酸不溶性灰分,可取供试品3~5g),置炽灼至恒重的坩埚中,称定重量(准确至0.01g),缓缓炽热,注意避免燃烧,至完全炭化时,逐渐升高温度至500~600℃,使完全灰化并至恒重。根据残渣重量,计算供试品中总灰分的含量(%)。结果判定:本品总灰分不得过15%。
重金属及有害元素
仪器及用具:中药粉碎机、分析天平、药典筛、微波消解仪、原子吸收分光光度计
试剂及试液:硝酸、磷酸二氢铵、硝酸镁、碘化钾、抗坏血酸、盐酸、硼氢化钠、氢氧化钠、硫酸、高锰酸钾、盐酸羟胺(其中硝酸、磷酸二氢铵、硝酸镁为优级纯,其他试剂均使用分析纯,实验用水为纯化水)
标准样品:铅单元素标准样品、镉单元素标准样品、砷单元素标准样品、汞单元素标准样品、铜单元素标准样品
方法:照铅、镉、砷、汞、铜测定法(通则2321)测定
铅的测定(石墨炉法)
测定条件 参考条件:波长283.3nm,干燥温度100~120℃,持续20秒;灰化温度400~750℃,持续20~25秒;原子化温度1700~~2100℃,持续4~5秒。
铅标准贮备液的制备 精密量取铅单元素标准溶液适量,用2%硝酸溶液稀释,制成每1ml含铅(Pb)1μg的溶液,即得(0~5℃贮存)。
标准曲线的制备 分别精密量取铅标准贮备液适量,用2%硝酸溶液制成每1ml分别含铅0ng、5ng、20ng、40ng、60ng、80ng的溶液。分别精密量取1ml,精密加含1%磷酸二氢铵和0.2%硝酸镁的溶液0.5ml,混匀,精密吸取20μl注入石墨炉原子化器,测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线。
供试品溶液的制备A法 取供试品粗粉0.5g,精密称定,置聚四氯乙烯消解罐内,加硝酸3~5ml,混匀,浸泡过夜,盖好内盖,旋紧外套,置适宜的微波消解炉内,进行消解(按仪器规定的消解程序操作)。消解完全后,取消解内罐置电热板上缓缓加热至红棕色蒸气挥尽,并继续缓缓浓缩至2~3ml,放冷,用水转入25ml量瓶中,并稀释至刻度,摇匀,即得。同法同时制备试剂空白溶液。
测定法 精密量取空白溶液与供试品溶液各1ml,精密加含1%磷酸二氢铵和0.2%硝酸镁的溶液0.5ml,混匀,精密吸取10~20μl,照标准曲线的制备项下方法测定吸光度,从标准曲线上读出供试品溶液中铅(Pb)的含量,计算,即得。
镉的测定(石墨炉法)
测定条件 参考条件:波长228.8nm,干燥温度100~120℃,持续20秒;灰化温度300~500℃,持续20~25秒;原子化温度1500~1900℃,持续4~5秒。
镉标准贮备液的制备精密量取镉单元素标准溶液适量,用2%硝酸溶液稀释,制成每1ml含镉(Cd)1μg的溶液,即得(0~5℃贮存)。
标准曲线的制备 分别精密量取镉标准贮备液适量,用2%硝酸溶液稀释制成每1ml分别含镉0ng、0.8ng、2.0ng、4.0ng、6.0ng、8.0ng的溶液。分别精密吸取10μl,注入石墨炉原子化器,测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线。
供试品溶液的制备 同铅测定项下供试品溶液的制备。
测定法精密吸取空白溶液与供试品溶液各10~20μl,照标准曲线的制备项下方法测定吸光度(若供试品有干扰,可分别精密量取标准溶液、空白溶液和供试品溶液各1ml,精密加含1%磷酸二氢铵和0.2%硝酸镁的溶液0.5ml,混匀,依法测定),从标准曲线上读出供试品溶液中镉(Cd)的含量,计算,即得。
砷的测定(氢化物法)
测定条件 采用适宜的氢化物发生装置,以含硼氢化钠和0.3%氢氧化钠溶液(临用前配制)作为还原剂,盐酸溶液(1→100)为载液,氮气为载气,检测波长为193.7nm。
砷标准贮备液的制备 精密量取砷单元素标准溶液适量,用2%硝酸溶液稀释,制成每1ml含砷(As)1μg的溶液,即得(0~5℃贮存)。
标准曲线的制备 分别精密量取砷标准贮备液适量,用2%硝酸溶液稀释制成每1ml分别含砷0ng、5ng、10ng、20ng、30ng、40ng的溶液。分别精密量取10ml,置25ml量瓶中,加25%碘化钾溶液(临用前配制)1ml,摇匀,加10%抗坏血酸溶液(临用前配制)1ml,摇匀,用盐酸溶液(20→100)稀释至刻度,摇匀,密塞,置80℃水浴中加热3分 钟,取出,放冷。取适量,吸入氢化物发生装置,测定吸收值,以峰面积(或吸光度)为纵坐标,浓度为横坐标,绘制标准曲线。
供试品溶液的制备 同铅测定项下供试品溶液的制备中的A法制备。
测定法 精密吸取空白溶液与供试品溶液各10ml,照标准曲线的制备项下,自“加25%碘化钾溶液(临用前配制)1ml”起,依法测定。从标准曲线上读出供试品溶液中砷(As)的含量,计算,即得。
汞的测定(冷蒸气吸收法)
测定条件 采用适宜的氢化物发生装置,以含0.5%硼氢化钠和0.1%氢氧化钠的溶液(临用前配制)作为还原剂,盐酸溶液(1→100)为载液,氮气为载气,检测波长为253.6nm。
汞标准贮备液的制备 精密量取汞单元素标准溶液适量,用2%硝酸溶液稀释,制成每1ml含汞(Hg)1μg的溶液,即得(0~5℃贮存)。
标准曲线的制备 分别精密量取汞标准贮备液0ml、0.1ml、0.3ml、0.5ml、0.7ml、0.9ml,置50ml量瓶中,加20%硫酸溶液10ml、5%高锰酸钾溶液0.5ml,摇匀,滴加5%盐酸羟胺溶液至紫红色恰消失,用水稀释至刻度,摇匀。取适量,吸入氢化物发生装置,测定吸收值,以峰面积(或吸光度)为纵坐标,浓度为横坐标,绘制标准曲线。
供试品溶液的制备A法 取供试品粗粉0.5g,精密称定,置聚四氟乙烯消解罐内,加硝酸3~5ml,混匀,浸泡过夜,盖好内盖,旋紧外套,置适宜的微波消解炉内进行消解(按仪器规定的消解程序操作)。消解完全后,取消解内罐置电热板上,于120℃缓缓加热至红棕色蒸气挥尽,并继续浓缩至2~3ml,放冷,加20%硫酸溶液2ml、5%高锰酸钾溶液0.5ml,摇匀,滴加5%盐酸羟胺溶液至紫红色恰消失,转入10ml量瓶中,用水洗涤容器,洗液合并于量瓶中,并稀释至刻度,摇匀,必要时离心,取上清液,即得。同法同时制备试剂空白溶液。
测定法 精密吸取空白溶液与供试品溶液适量,照标准曲线制备项下的方法测定从标准曲线上读出供试品溶液中汞(Hg)的含量,计算,即得。
铜的测定(火焰法)
测定条件 检测波长为324.7nm,采用空气-乙炔火焰,必要时进行背景校正。
铜标准贮备液的制备 精密量取铜单元素标准溶液适量,用2%硝酸溶液稀释,制成每1ml含铜(Cu)10μg的溶液,即得(0~5℃贮存)。
标准曲线的制备 分别精密量取铜标准贮备液适量,用2%硝酸溶液制成每1ml分别含铜0μg、0.05μg、0.2μg、4μg、0.6μg、0.8μg的溶液。依次喷入火焰,测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线。
供试品溶液的制备 同铅测定项下供试品溶液的制备。
测定法 精密吸取空白溶液与供试品溶液适量,照标准曲线的制备项下的方法测定。从标准曲线上读出供试品溶液中铜(Cu)的含量,计算,即得。
结果判定:本品含铅不得过8mg/kg、镉不得过0.8mg/kg、砷不得过4mg/kg、汞不得过0.8mg/kg、铜不得过20mg/kg。
有机氯类农药残留量
仪器及用具:中药粉碎机、分析天平、药典筛、旋转蒸发仪、超声波清洗机、气相色谱仪
试剂及试液:石油醚(60~90℃)、丙酮、氯化钠、二氯甲烷、无水硫酸钠(其中石油醚(60~90℃)为色谱纯,其他试剂均使用分析纯,实验用水为纯化水)
对照品:α-BHC,β-BHC,γ-BHC,δ-BHC、pp′-DDE,pp′-DDD,op′-DDT,pp′-DDT、PCNB农药对照品
方法:照农药残留量测定法(通则0512第一法)测定。
色谱条件与系统适用性试验 以(14%-氰丙基-苯基)甲基聚硅氧烷或(5%苯基)甲基聚硅氧烷为固定液的弹性石英毛细管柱(30m×0.32mm×0.25μm),63Ni-ECD电子捕获检测器。进样口温度230℃,检测器温度300℃,不分流进样。程序升温:初始100℃,每分钟10℃升至220℃,每分钟8℃升至250℃,保持10分钟。理论板数按α-BHC峰计算应不低于1×106,两个相邻色谱峰的分离度应大于1.5。
对照品贮备溶液的制备精密称取六六六(BHC)(α-BHC,β-BHC,γ-BHC,δ-BHC)、滴滴涕(DDT)(pp′-DDE,pp′-DDD,op′-DDT,pp′-DDT)及五氯硝基苯(PCNB)农药对照品适量,用石油醚(60~90℃)分别制成每1ml约含4~5μg的溶液,即得。
混合对照品贮备溶液的制备 精密量取上述各对照品贮备液0.5ml,置10ml量瓶中,用石油醚(60~90℃)稀释至刻度,摇匀,即得。
混合对照品溶液的制备 精密量取上述混合对照品贮备液,用石油醚(60~90℃)制成每1L分别含0μg、1μg、5μg、10μg、50μg、100μg、250μg的溶液,即得。
供试品溶液的制备 取供试品,粉碎成粉末(过三号筛),取约2g,精密称定,置100ml具塞锥形瓶中,加水20ml浸泡过夜,精密加丙酮40ml,称定重量,超声处理30分钟,放冷,再称定重量,用丙酮补足减失的重量,再加氯化钠约6g,精密加二氯甲烷30ml,称定重量,超声15分钟,再称定重量,用二氯甲烷补足减失的重量,静置(使分层),将有机相迅速移入装有适量无水硫酸钠的100ml具塞锥形瓶中,放置4小时。精密量取35ml,于40℃水浴上减压浓缩至近干,加少量石油醚(60~90℃)如前反复操作至二氯甲烷及丙酮除净,用石油醚(60~90℃)溶解并转移至10ml具塞刻度离心管中,加石油醚(60~90℃)精密稀释至5ml,小心加入硫酸1ml,振摇1分钟,离心(3000转/分钟)10分钟,精密量取上清液2ml,置具刻度的浓缩瓶中,连接旋转蒸发器,40℃下(或用氮气)将溶液浓缩至适量,精密稀释至1ml,即得。
测定法 分别精密吸取供试品溶液和与之相对应浓度的混合对照品溶液各1μl,注入气相色谱仪,按外标法计算供试品中9种有机氯农药残留量。
结果判定:本品含总六六六(α-BHC、β-BHC、γ-BHC、δ-BHC之和)不得过0.2mg/kg、总滴滴涕(pp′-DDE、pp′-DDD、op′-DDT、pp′-DDT之和)不得过0.2mg/kg、五氯硝基苯不得过0.1mg/kg。
黄曲霉毒素B1
仪器及用具:中药粉碎机、分析天平、药典筛、均质瓶、离心机、高效液相色谱仪(配置荧光检测器及衍生化泵、衍生化保温箱)
试剂及试液:甲醇、乙腈、碘、氯化钠、免疫亲合柱(其中乙腈为色谱纯,其他试剂为分析纯,实验用水为纯化水)
对照品:黄曲霉毒素B1对照品
方法:照黄曲霉毒素测定法(通则2351)测定。
色谱条件与系统适用性试验 以十八烷基硅烷键合硅胶为填充剂;以甲醇-乙腈-水(40∶18∶42)为流动相;采用柱后衍生法检测,碘衍生法:衍生溶液为0.05%的碘溶液(取碘0.5g,加入甲醇100ml使溶解,用水稀释至1000ml制成),衍生化泵流速每分钟0.3ml,衍生化温度70℃以荧光检测器检测,激发波长λex=360nm(或365nm),发射波长λex=450nm。两个相邻色谱峰的分离度应大于1.5。
混合对照品溶液的制备 精密量取黄曲霉毒素B1对照品溶液(标示浓度为1.0μg/ml)0.5ml,置10ml量瓶中,用甲醇稀释至刻度,作为贮备溶液。精密量取贮备溶液1ml,置25ml量瓶中,用甲醇稀释至刻度,即得。
供试品溶液的制备取供试品粉末约15g(过二号筛),精密称定,置于均质瓶中,加入氯化钠3g,精密加入70%甲醇溶液75ml,高速搅拌2分钟(搅拌速度大于11000转/分钟),离心5分钟(离心速度2500转/分钟),精密量取上清液15ml,置50ml量瓶中,用水稀释至刻度,摇匀,用微孔滤膜(0.45μm)滤过,量取续滤液20.0ml,通过免疫亲合柱,流速每分钟3ml,用水20ml洗脱,洗脱液弃去,使空气进入柱子,将水挤出柱子,再用适量甲醇洗脱,收集洗脱液,置2ml量瓶中,并用甲醇稀释至刻度,摇匀,即得。
测定法 分别精密吸取上述混合对照品溶液5μl、10μl、15μl、20μl、25μl,注入液相色谱仪,测定峰面积,以峰面积为纵坐标,进样量为横坐标,绘制标准曲线。另精密吸取上述供试品溶液20~25μl,注入液相色谱仪,测定峰面积,从标准曲线上读出供试品中相当于黄曲霉毒素B1的量,计算,即得。
结果判定:本品每1000g含黄曲霉毒素B1不得过5μg。
二氧化硫残留量
仪器及用具:中药粉碎机、分析天平、药典筛、电热套
试剂及试液:过氧化氢、甲基红乙醇溶液、0.01mol/L氢氧化钠滴定液、盐酸溶液(6mol/L)(试剂均使用分析纯,实验用水为纯化水)
方法:照二氧化硫残留量测定法(通则2331)测定。取药材或饮片细粉约10g,精密称定,置两颈圆底烧瓶中,加水300~400ml。打开回流冷凝管开关给水,将冷凝管的上端E口处连接一橡胶导气管置于100ml锥形瓶底部。锥形瓶内加入3%过氧化氢溶液50ml作为吸收液(橡胶导气管的末端应在吸收液液面以下)。使用前,在吸收液中加入3滴甲基红乙醇溶液指示剂(2.5mg/ml),并用0.01mol/L氢氧化钠滴定液滴定至黄色(即终点;如果超过终点,则应舍弃该吸收溶液)。开通氮气,使用流量计调节气体流量至约0.2L/min;打开分液漏斗C的活塞,使盐酸溶液(6mol/L)10ml流入蒸馏瓶,立即加热两颈烧瓶内的溶液至沸,并保持微沸;烧瓶内的水沸腾1.5小时后,停止加热。吸收液放冷后,置于磁力搅 拌器上不断搅拌,用氢氧化钠滴定液(0.01mol/L)滴定,至黄色持续时间20秒不褪,并将滴定的结果用空白实验校正。
结果判定:本品二氧化硫残留量不得过150mg/kg。
浸出物
仪器及用具:中药粉碎机、分析天平、药典筛、恒温水浴锅、电热恒温鼓风干燥箱
试剂及试液:乙醇(试剂使用分析纯,实验用水为纯化水)
方法:醇溶性浸出物,照醇溶性浸出物测定法(通则2201)项下的热浸法测定,用乙醇作溶剂。
热浸法 取供试品约2~4g,精密称定,置100~250ml的锥形瓶中,精密加乙醇50~100ml,密塞,称定重量,静置1小时后,连接回流冷凝管,加热至沸腾,并保持微沸1小时。放冷后,取下锥形瓶,密塞,再称定重量,用乙醇补足减失的重量,摇匀,用干燥滤器滤过,精密量取滤液25ml,置已干燥至恒重的蒸发皿中,在水浴上蒸干后,于105℃干燥3小时,置干燥器中冷却30分钟,迅速精密称定重量。除另有规定外,以干燥品计算供试品中醇溶性浸出物的含量(%)。
结果判定:本品醇溶性浸出物不得少于7.0%。
含量测定
仪器及用具:中药粉碎机、分析天平、药典筛、超声波清洗机、高效液相色谱仪
试剂及试液:甲醇、磷酸、三氯甲烷(其中甲醇为色谱纯,其他试剂为分析纯,实验用水为纯化水)
对照品:野黄芩苷对照品
方法:照高效液相色谱法(通则0512)测定。
色谱条件与系统适用性试验以十八烷基硅烷键合硅胶为填充剂;以甲醇-0.1%磷酸溶液(40∶60)为流动相;检测波长为335nm。理论板数按野黄芩苷峰计算应不低于5000。
对照品溶液的制备 取野黄芩苷对照品适量,精密称定,加甲醇制成每1ml含0.1mg的溶液,即得。
供试品溶液的制备 取本品粗粉约0.5g,精密称定,置索氏提取器中,加三氯甲烷适量,加热回流至提取液无绿色,弃去三氯甲烷液,药渣挥去溶剂,连同滤纸筒移入具塞锥形瓶中,精密加入甲醇50ml,密塞,称定重量,放置1小时,水浴中加热回流1小时,放冷,再称定重量,用甲醇补足减失的重量,摇匀,滤过。精密量取续滤液25ml,回收溶剂至干,残渣用甲醇溶解并转移至10ml量瓶中,加甲醇至刻度,摇匀,滤过,取续滤液,即得。
测定法 分别精密吸取对照品溶液与供试品溶液各5~10μl,注入液相色谱仪,测定,即得。
结果判定:本品按干燥品计算,含野黄芩苷(C21H18O12)不得少于0.33%。
微生物限度
沙门菌 取本品10g,以无菌接种至适宜体积(经方法适用性实验确定)的胰酪大豆胨液体培养基中,混匀,按非无菌产品微生物限度检查:控制菌检查法检查。
结果判定:沙门菌不得检出(10g)。
耐胆盐革兰阴性菌取本品,以无菌胰酪大豆胨液体培养基为稀释剂,制成1∶10的供试液,混匀,按非无菌产品微生物限度检查:控制菌检查法检查。
结果判定:耐胆盐革兰阴性菌应小于104cfu(1g)。
Claims (3)
1.灯盏花定性定量中药饮片的质量标准,其特征在于:在现行版《中国药典》质量标准的基础上增加药屑杂质、重金属及有害元素、黄曲霉毒素B1、二氧化硫残留量,并将含量测定中的野黄芩苷总量的标准限度从0.30%提高至0.33%。
2.如权利要求1中所述的灯盏花定性定量中药饮片的质量标准,其特征在于:
药屑杂质照杂质检查法(《中国药典》2015年版四部通则2301)测定(《中国药典》2015年版四部通则以下简称通则),应不得过3%。
重金属及有害元素照铅、镉、砷、汞、铜测定法(通则2321)测定,本品含铅不得过8mg/kg、镉不得过0.8mg/kg、砷不得过4mg/kg、汞不得过0.8mg/kg、铜不得过20mg/kg。
黄曲霉毒素B1照黄曲霉毒素测定法(通则2351)测定,本品含黄曲霉毒素B1不得过5μg/kg。
二氧化硫残留量照二氧化硫残留量测定法(通则2331)测定,本品二氧化硫残留量不得过150mg/kg。
3.灯盏花定性定量中药饮片的制造工艺,其特征在于制备出灯盏花中药饮片,包括以下步骤:
A10、净制:清除混在药物中的杂质及霉变品等,或将药物按大小进行分档,以便达到洁净或进一步加工处理。
A20、润药:净制后的药材放入洗润池中,喷水堆润6-8h,至药材彻底润透。
A30、切制:按全自动高速切片机操作规程操作,调好刀距0.4mm,进行切药。
A40、干燥:采用热风循环烘箱进行干燥,将药材铺于烘箱架子上,摊铺厚度均匀,厚度在3cm以下。打开开关,开启加热开关、风机,在温度60±2℃进行干燥,在温度达到设定温度后干燥5-7h,干燥完毕,关闭加热开关,继续吹风,待箱内温度降下至35~40℃,关闭风机。干燥后岗位人员需填写中间产品请检单,交质量部由QA取样进行水分检查。
A50、包装:根据本品包装规格要求进行包装。包装前需对包装间进行检查,确认包装生产线的清场已经完成,并核对包装材料是否符合要求。内包装:在设备上调整好需要印制的生产日期、批号,QA监控,称取规定重量的药材放入料斗中,用封口机封口,要求做到封口严密、平整、美观外包装:在设备上调整好需印制的生产日期及批号,QA监控,在外包装盒子上打印批号、生产日期,打印过程中需注意批号及生产日期是否清晰。将内包装完成后的饮片及检验报告书放入外包盒中,4袋/盒。将每10盒饮片,套入1个热缩膜中,进行热收缩;热收缩后装入大纸箱中,240盒/箱。操作过程中,QA随时抽检。
A60、成品:包装后岗位人员需填写成品请检单,交质量部由QA取样进行产品检查。
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