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中国药典2015版/2020版0982 粒度和粒度分布测定法-515

ZHONGGUOYAODIAN2015BAN/2020BAN0982 LIDUHELIDUFENBUCEDINGFA-515

BENFAYONGYUCEDINGYUANLIAOYAOHEYAOWUZHIJIDELIZIDAXIAOHUOLIDUFENBU。QIZHONGDIYIFA、DIERFAYONGYUCEDINGYAOWUZHIJIDELIZIDAXIAOHUOXIANDU,DISANFAYONGYUCEDINGYUANLIAOYAOHUOYAOWUZHIJIDELIDUFENBU。

  1. 空气喷射筛分法

MEICISHAIFENSHIJINSHIYONGYIGEYAOSHAI。RUXUCEDINGKELIDAXIAOFENBU,YINGCONGKONGJINGZUIXIAODEYAOSHAIKAISHISHUNXUJINXING。 CHULINGYOUGUIDINGWAI,QUZHIJINGWEI200mmGUIDINGHAODEYAOSHAI,CHENGDINGZHONGLIANG,GENJUGONGSHIPINDERONGJIMIDU,CHENGQUGONGSHIPIN25~100g,ZHIYAOSHAIZHONG,SHAISHANGJIAGAI。SHEDINGYALI,PENSHE5FENZHONG。QUYAOSHAI,CHENGDINGZONGLIANG,GENJUSHAIFENQIANHOUDEZHONGLIANGCHAYIJISUANYAOSHAISHANGKELIJIFENMOSUOZHANBILI(%)。ZHONGFUSHANGSHUCAOZUOZHIZHILIANXULIANGCISHAIFENHOU,YAOSHAISHANGYILIUKELIJIFENMOZHONGLIANGDECHAYIBUCHAOGUOQIANCIYILIUKELIJIFENMOZHONGLIANGDE5%HUOLIANGCIZHONGLIANGDECHAZHIBUDAYU0.1g; RUOYAOSHAISHANGYILIUDEKELIJIFENMOZHONGLIANGXIAOYUGONGSHIPINQUYANGLIANGDE5%,ZELIANXULIANGCIDEZHONGLIANGCHAYIYINGBUCHAOGUO20%。

汇美科HMK-200空气喷射筛

第一法(显微镜法)

BENFAZHONGDELIDU,XIYIXIANWEIJINGXIAGUANCHADAODEZHANGDUBIAOSHI。

目镜测微尺的标定  照显微鉴别法(通则2001)标定目镜测微尺。

测定法  取供试品,用力摇匀,粘度较大者可按各种项下的规定加适量甘油溶液(1→2)稀释,照该剂型或各品种项下的规定,量取供试品,置载玻璃片上,覆以盖玻片,轻压使颗粒分布均匀,注意防止气泡混入,半固体可直接涂在载玻璃片上,立即在50~100倍显微镜下检视盖玻片全部视野,应无凝聚现象,并不得检出该剂型或各品种项下规定的50μm及以上的粒子。再在200~500倍的显微镜下检视该剂型或各品种项下规定的视野内的总粒数及规定大小的粒数,并计算其所占比例(%)。

第二法(筛分法)

SHAIFENFAYIBANFENWEISHOUDONGSHAIFENFA、JIXIESHAIFENFAYUKONGQIPENSHESHAIFENFA。SHOUDONGSHAIFENFAHEJIXIESHAIFENFASHIYONGYUCEDINGDABUFENLIJINGDAYU75μmDEYANGPIN。DUIYULIJINGXIAOYU75μmDEYANGPIN,ZEYINGCAIYONGKONGQIPENSHESHAIFENFAHUOQITASHIYIDEFANGFA。

JIXIESHAIFENFAXICAIYONGJIXIEFANGFAHUODIANCIFANGFA,CHANSHENGCHUIZHIZHENDONG、SHUIPINGYUANZHOUYUNDONG、PAIDA、PAIDAYUSHUIPINGYUANZHOUYUNDONGXIANGJIEHEDENGZHENDONGFANGSHI。KONGQIPENSHESHAIFENFAZECAIYONGLIUDONGDEKONGQILIUDAIDONGKELIYUNDONG。

SHAIFENSHIYANSHIXUZHUYIHUANJINGSHIDU,FANGZHIYANGPINXISHUIHUOSHISHUI。DUIYICHANSHENGJINGDIANDEYANGPIN,KEJIARU0.5%JIAOZHIERYANGHUAGUIHE(HUO)YANGHUALVDENGKANGJINGDIANJI,YIJIANXIAOJINGDIANZUOYONGCHANSHENGDEYINGXIANG。

  1. 手动筛分法
  • 单筛分法 称取各品种项下规定的供试品,置规定号的药筛中(筛下配有密合的接收容器),筛上加盖。按水平方向旋转振摇至少3分钟,并不时在垂直方向轻叩筛。取筛下的颗粒及粉末,称定重量,计算其所占比例(%)。
  • 双筛分法 取单剂量包装的5袋(瓶)或多剂量包装的1袋(瓶),称定重量,置该剂型或品种项下规定的上层(孔径大的)药筛中(下层的筛下配有密合的接收容器),保持水平状态过筛,左右往返,边筛动边拍打3分钟。取不能通过大孔径筛和能通过小孔径筛的颗粒及粉末,称定重量,计算其所占比例(%)。
  1. 机械筛分法

CHULINGYOUGUIDINGWAI,QUZHIJINGWEI200mmGUIDINGHAODEYAOSHAIHEJIESHOURONGQI,CHENGDINGZHONGLIANG,GENJUGONGSHIPINDERONGJIMIDU,CHENGQUGONGSHIPIN25~100g,ZHIZUISHANGCENG(KONGJINGZUIDADE)YAOSHAIZHONG(ZUIXIACENGDESHAIXIAPEIYOUMIHEDEJIESHOURONGQI),SHAISHANGJIAGAI。SHEDINGZHENDONGFANGSHIHEZHENDONGPINLV,ZHENDONG5FENZHONG。QUGEYAOSHAIYUJIESHOURONGQI,CHENGDINGZHONGLIANG,GENJUSHAIFENQIANHOUDEZHONGLIANGCHAYIJISUANGEYAOSHAISHANGHEJIESHOURONGQINEIKELIJIFENMOSUOZHANBILI(%)。ZHONGFUSHANGSHUCAOZUOZHIZHILIANXULIANGCISHAIFENHOU,GEYAOSHAISHANGYILIUKELIJIFENMOZHONGLIANGDECHAYIBUCHAOGUOQIANCIYILIUKELIJIFENMOZHONGLIANGDE5%HUOLIANGCIZHONGLIANGDECHAZHIBUDAYU0.1g; RUOMOUYIYAOSHAISHANGYILIUKELIJIFENMODEZHONGLIANGXIAOYUGONGSHIPINQUYANGLIANGDE5%,ZEGAIYAOSHAILIANXULIANGCIDEZHONGLIANGCHAYIYINGBUCHAOGUO20%。

(NEIRONGQINGJIANWENZHANGKAISHIBUFEN)

第三法(光散射法)

DANSEGUANGSHUZHAOSHEDAOKELIGONGSHIPINHOUJIFASHENGSANSHEXIANXIANG。YOUYUSANSHEGUANGDENENGLIANGFENBUYUKELIDEDAXIAOYOUGUAN,TONGGUOCELIANGSANSHEGUANGDENENGLIANGFENBU(SANSHEJIAO),YIJUMISHISANSHELILUNHEFULANGHUOFUJINSILILUN,JIKEJISUANCHUKELIDELIDUFENBU。BENFADECELIANGFANWEIKEDA0.02~3500μm。SUOYONGYIQIWEIJIGUANGSANSHELIDUFENBUYI。

 

  1. 对仪器的一般要求

散射仪  光源发出的激光强度应稳定,并且能够自动扣除电子背景和光学背景等的干扰。

CAIYONGLIJINGFENBUTEZHENGZHI[d(0.1)、d(0.5)、d(0.9)]YIZHIDE“BIAOZHUNLIZI”DUIYIQIJINXINGPINGJIA。TONGCHANGYONGXIANGDUIBIAOZHUNPIANCHA(RSD)BIAOZHENG“BIAOZHUNLIZI”DELIJINGFENBUFANWEI,DANGRSD XIAOYU50%(ZUIDALIJINGYUZUIXIAOLIJINGDEBILVYUEWEI10:1)SHI,PINGXINGCEDING5CI,“BIAOZHUNLIZI”DEd (0.5) JUNZHIYUQITEZHENGZHIDEPIANCHAYINGXIAOYU3%,PINGXINGCEDINGDERSDBUDEGUO3%;“BIAOZHUNLIZI”DEd (0.1)HEd(0.9)JUNZHIYUQITEZHENGZHIDEPIANCHAJUNYINGXIAOYU5%,PINGXINGCEDINGDERSDJUNBUDEGUO5%;DUILIJINGXIAOYU10μmDE“BIAOZHUNLIZI”,CEDINGDEd(0.5)JUNZHIYUQITEZHENGZHIDEPIANCHAYINGXIAOYU6%,PINGXINGCEDINGDERSDBUDEGUO6%;d(0.1)HEd(0.9)DEJUNZHIYUQITEZHENGZHIDEPIANCHAJUNYINGXIAOYU10%,PINGXINGCEDINGDERSDJUNBUDEGUO10%。

  1. 测定法

GENJUGONGSHIPINDEXINGZHUANGHERONGJIEXINGNENG,XUANZESHIFACEDINGHUOGANFACEDING;SHIFACEDINGYONGYUCEDINGHUNXUANGONGSHIPINHUOBURONGYUFENSANJIEZHIDEGONGSHIPIN,GANFACEDINGYONGYUCEDINGSHUIRONGXINGHUOWUSHIHEFENSANJIEZHIDEGUTAIGONGSHIPIN。

湿法测定  湿法测定的检测下限通常为20nm。

GENJUGONGSHIPINDETEXING,XUANZESHIYIDEFENSANFANGFASHIGONGSHIPINFENSANCHENGWENDINGDEHUNXUANYE;TONGCHANGKECAIYONGWULIFENSANDEFANGFARUCHAOSHENG、JIAOBANDENG,TONGGUODIAOJIECHAOSHENGGONGLVHEJIAOBANSUDU,BIYAOSHIKEJIARUSHILIANGDEHUAXUEFENSANJIHUOBIAOMIANHUOXINGJI,SHIFENSANTIXICHENGWENDINGZHUANGTAI,YIBAOZHENGGONGSHIPINNENGGOUJUNYUNWENDINGDITONGGUOJIANCECHUANGKOU, DEDAOZHUNQUEDECEDINGJIEGUO。

ZHIYOUDANGFENSANTIXIDESHUANGCENGDIANWEI(ζDIANWEI)CHUYUYIDINGFANWEINEI,TIXICAICHUYUWENDINGZHUANGTAI,YINCI,ZAIZHIBEIGONGSHIPINDEFENSANTIXISHI,YINGZHUYICELIANGTIXIζDIANWEI,YIBAOZHENGFENSANTIXIDEZHONGXIANXING。

SHIFACELIANGSUOXUYAODEGONGSHIPINLIANGTONGCHANGYINGDADAOJIANCEQIZHEGUANGDUFANWEIDE8%~20%;ZUIXIANJINDEJIGUANGLIDUYIDUIZHEGUANGDUDEXIAXIANYAOQIUKEDIZHI0.2%。

干法测定  干法测定的检测下限通常为200nm。

TONGCHANGCAIYONGMIBICELIANGFA,YIJIANSHAOGONGSHIPINXICHAO。XUANYONGDEGANFAJINYANGQIJIYANGPINCHIXUKEFUPIANLIUXIAOYING,GENJUGONGSHIPINFENSANDENANYI,DIAOJIEFENSANQIDEQILIUYALI,SHIBUTONGDAXIAODELIZIYITONGYANGDESUDUJUNYUNWENDINGDITONGGUOJIANCECHUANGKOU,YIDEDAOZHUNQUEDECEDINGJIEGUO。

DUIYUHUAXUEYUANLIAOYAO,YINGCAIYONGPENSHESHIFENSANQI。ZAIYANGPINPANZHONGXIANJIARUSHILIANGDEJINSHUXIAOQIU,ZAIJIARUGONGSHIPIN,DIAOJIEZHENDONGJINYANGSUDU、FENSANQIYA(TONGCHANGWEI0~0.4MPa)HEYANGPINCHUKOUDEXIAFENGKUANDU,YIKONGZHIGONGSHIPINDEFENSANCHENGDUHETONGGUOJIANCEQIDEGONGSHIPINLIANG。

GANFACELIANGSUOXUYAODEGONGSHIPINLIANGTONGCHANGYINGDADAOJIANCEQIZHEGUANGDUFANWEIDE0.5%~5%。

附注】(1)仪器光学参数的设置与供试品的粒度分布有关。粒径大于10μm的微粒,对系统折光率和吸光度的影响较小;粒径小于10μm的微粒,对系统折光率和吸光度的影响较大。在对不同原料和制剂的粒度进行分析时,目前还没有成熟的理论用于指导对仪器光学参数的设置,应有实验比较决定,并采用标准粒子对仪器进行校准。

(2)DUIYOUSEWUZHI、RUHUAYEHELIJINGXIAOYU10μmDEWUZHIJINXINGLIDUFENBUCELIANGSHI,WEILEJIANSHAOCELIANGWUCHA,YINGSHIYONGMISHILILUNJISUANJIEGUO,BIMIANSHIYONGYIFULANGHUOFUJINSILILUNWEIJICHUDEJISUANGONGSHI。

(3)DUILIJINGFENBUFANWEIJIAOKUANDEGONGSHIPINJINXINGCEDINGSHI,BUYICAIYONGFENDUANCELIANGDEFANGFA,ERYINGSHIYONGHANGAIZHENGGECELIANGFANWEIDEDANYILIANGCHENGJIANCEQI,YIJIANSHAOCELIANGWUCHA。


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