环球时报 冰块棉签塞pp视频过程_好看视频_1314酒色,1314酒色真的不错_简笔画教程网
考虑到这篇文章并不是《永劫无间》手游的广告,举例就到此为止吧。其实我倒是觉得,游戏里的础滨不管智能与否,都有种杀猪盘的感觉。表面上是人与人的互动,实则是深入学习了人类心理学的础滨人机,在你花钱的时候拍马屁,在你连败的时候送温暖,让你欲罢不能。
2024年12月29日,不仅是上证指数,如果仔细观察,沪深300和上证50,也是在周五放量了。
环球时报 冰块棉签塞pp视频过程_好看视频_1314酒色,1314酒色真的不错_简笔画教程网
朋友同事知道这个消息之后已经通知他在国内的父母并正在协助他们来美国处理后事
当然,“停车难”是大城市车主出行面临的共同问题。在“充电专用”的背景下,不排除部分新能源车主以充电为名,占用车位,实际上只是为了方便自己停车。因此,新能源汽车的免费停车时间应当是有限定的。不能让新能源车主“钻空子”,挤占稀缺的停车资源。说来说去,你就是嫌她半夜叁更打扰你,让你送我来医院是吧,累着你了是吧。
hahahahahahefeiyaohaiqu,tianzuo,shangchenghejiuzuotai,ruhexuanzene?yuanchuang2022-04-11 13:06·loushitansuozheyaohaiqu,jinqizuihaomaideloupan,suanshilonghutianzuoliao,zuotianpeifensikanliaosangeloupan,fenbieshilonghutianzuo,longhushangchengheweixingjiuzuotai。weishimefensizhiyuanyikanyaohaishiqudefangzine?diyi,xiguanliaozhoubiandeshenghuohuanjing,buyuanyizaixinanmaifang;dier,qinqipengyouduzaifujinjuzhu,ruguozhihuandefangzitaiyuanliao,jiaojiquanjiuhuibianxiao;disan,xinanbianjuligongsitaiyuanliao,shangbanfeichangbufangbian;disi,fensishifeidongren,buxiangzhihuanfangchanzhihou,huanshimailiaofeidongchanzhengdefangzi,suoyi,zhinengkankaojinshiqudexinfangliao。zongdelaishuo,zhegefensijiushidianxingdediyuanxinggoufangzhe。fensikanwanfangzizhihou,zuizhonghuanshixuanzegoumailonghutianzuoliao。weishimehuixuanzelonghutianzuo,erbushishangchenghejiuzuotaine?diyi,longhushangchengdeweizhibijiaozuozuo。loupanbeibianshibeierhuan,bingqie,xianzaigaojiaqiaoyetongcheliao,dongbianshitonglinglugaojiaqiao,nanbianshihuochedao,dajiakenengduzhidao,huochedaodezaoyinbusuanda,checibijiaoshao,sudubijiaokuai,ergaojiaqiaodezaoyinshixiangdangdade,keyishuowushiwukebuzaichuanchujudadezaoyin。loupanxibianshiyaohaijiajucheng,zhoubianhuanyoudaliangdesiSdian,keyishuo,congzhoubianhuanjinglaikan,haowuliangdian。congjiaotongshanglaikan,juliditiezhanbijiaoyuan,erjulihuochezhanjulijin,bujinbushiyouxiaopeitao,huanshuyuyouhaipeitao,zheyidian,wozaizhiqiandefabudewenzhangyouxiangxidefenxi。zaicongfangjiashanglaikan,shangchengdejunjia20500yuanzuoyoumeipingmi,duibizhoubiandeershoufangjiage,shuyuxinfangjiageyuanyuangaoyuershoufangjiage,ruguomailiaofangzi,yihouxiangmaichudeshihou,jiageshangjiuhennanyoushimeyoushiliao,ermaifangkaolvdediyiyaosujiushifangchandeshengzhikongjian。shangchengdeyoudian,yejiushiloupanbenshendepinpaihewuye,longhuzuijinliangnian,zaihefeidefangdichanshichangzhong,koubeizuodexiangdangbucuo。shangchengchuliaozishendepinpaihewuyezhiwai,qitafangmiandumeiyoushimemingxiandeliangdian。dier,weixingjiuzuotai,dongbianxinzhongxinhexinbankuaiweiyizaishouxinpan。youdian:congdiduanshanglaishuo,jiuzuotaishuyuhefeishishisiwuguihuazhong“yiqusiji”zhongdeyiji,qidingweishixiangdanggaode,weilaidefazhankongjianjuda;jiuzuotaizidai6.9wanfangshangyeti,ditieliuhaoxianzhijieduijieshangyeti,ditiechuxinghuifeichangfangbian,zhoubianhuanyoudaijiangongyuan,huanjingyehuibucuo;jiuzuotaidefangzibenshenyebucuo,zhuangxiuxijiefangmianfeichangzhoudao。jiagefangmianlaishuo,xingjiabibucuo,dongbuxinzhongxinhexindiduandepinzhiloupan,maopibeianjia17000zuoyou,jiashangliangqianyipingmidejingzhuangbao,junjiayiwanjiuqianduo,jiagefangmiancunzaibucuodeyoushi。suizhuodongbuxinzhongxindekaishijiakuai,houqidehuanjinghuiyuelaiyuehao,peitaoyuelaiyuehao,houqijuyoubucuodeshengzhikongjian。quedian:muqianyinweichuyukaifachushijieduan,zhoubiandepeitaohehuanjingdubushihenlixiang;xuequshidongfengxiaoxuehewushiwuzhongxue,xuequfangmianyiban;loupanbeibianshiyuxilugaojiaqiaohexinzhouguduipifashichang,huochelaiwangjiaoduo,nanbianshihuiqiananzhifang,waiweihuanjingbijiaozaluan。henduorenmaifang,zhikanduanqi,hennanhuikandaochangqidefazhan,suoyi,jiuzuotaidequhualvyebushihengao。disan,longhutianzuo。longhutianzuojieheliaoshangchenghejiuzuotaideyoudian,dangran,yecunzaimingxiandequedian。youdian:longhupinpaihelonghuwuyedejiachi;jiaotongbijiaobianli,ditieerhaoxianjiuzaixiaoqumenkou,changjianglushangdegongjiaochexianluyefeichangduo;zhoubiandeshangyeyebijiaoduo,yaohaiwandaguangchang,baolidongchengguangchang,baolidongjunhuanyouxiaoqubeibiandeyonghuichaoshihexiaoquxibiandelianjiachaoshi;xinfangjiagezaiyouyidingdedaogua,tianzuoxinfangyibanloucengdejiagezai18000dao19000zhijian,jiashang1000yuanmeipingmidejingzhuangbao,junjiayezai20000wanzhinei,erzhoubiandecixinfangjiageduzai20000yishangliao,houqixiangmaidiaotianzuodefangzi,shibucuoshouyide。quedian:changjiangdongludecheliuliangda,bingqie,huochebijiaoduo;xiaoqunanbianjiushichangjiangpifashichang,huoche,sanlunche,dianpingchetebieduo,bingqie,zhoubiandushifanglingjiaolaodexiaoqu,loupandewaiweihuanjingbijiaozangluan。zongjie:congsangeloupandezhengtiquhualvjiunenghenqingxidikanchulai,sangeloupanzhong,longhutianzuoshizuihaomaideloupanliao,longhutianzuoxianzaizhiyoushaoliangdediloucenghuxingzaishou,yinggaihenkuaijiunengqingpan;longhushangchengdequhualvbijiaodi,houqidequhuasuduyinggaibijiaoman;erweixingjiuzuotaijiujiandanliao,quniankaipan,xianzailoupanyijingquanbufengding,huanyoudaliangdefangyuandaishou,kejianquhuashibulixiangde。guanzhuloushitansuozhe,dainiliaojiegengduodefangchanzhishi,rangnimaifangshaozouwanlu。
NY/T 4307-2023 葛(Ge)根(Gen)中(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)的(De)测(Ce)定(Ding) 高(Gao)效(Xiao)液(Ye)相(Xiang)色(Se)谱(Pu)-串(Chuan)联(Lian)质(Zhi)谱(Pu)法(Fa)2023-12-20 08:43·xinpulai中(Zhong)华(Hua)人(Ren)民(Min)共(Gong)和(He)国(Guo)农(Nong)业(Ye)行(Xing)业(Ye)标(Biao)准(Zhun)NY/T 4307-2023葛(Ge)根(Gen)中(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)的(De)测(Ce)定(Ding)高(Gao)效(Xiao)液(Ye)相(Xiang)色(Se)谱(Pu)-串(Chuan)联(Lian)质(Zhi)谱(Pu)法(Fa)Determination of flavonoids in the root of kudzu vine-High performance liquid chromatography-mass spectrometry (HPLC-MS)前(Qian)言(Yan)本(Ben)文(Wen)件(Jian)按(An)照(Zhao)GB/T 1. 1-2020《标(Biao)准(Zhun)化(Hua)工(Gong)作(Zuo)导(Dao)则(Ze)第(Di)1部(Bu)分(Fen):标(Biao)准(Zhun)化(Hua)文(Wen)件(Jian)的(De)结(Jie)构(Gou)和(He)起(Qi)草(Cao)规(Gui)则(Ze)》的(De)规(Gui)定(Ding)起(Qi)草(Cao)。请(Qing)注(Zhu)意(Yi)本(Ben)文(Wen)件(Jian)的(De)某(Mou)些(Xie)内(Nei)容(Rong)可(Ke)能(Neng)涉(She)及(Ji)专(Zhuan)利(Li)。本(Ben)文(Wen)件(Jian)的(De)发(Fa)布(Bu)机(Ji)构(Gou)不(Bu)承(Cheng)担(Dan)识(Shi)别(Bie)专(Zhuan)利(Li)的(De)责(Ze)任(Ren)。本(Ben)文(Wen)件(Jian)由(You)农(Nong)业(Ye)农(Nong)村(Cun)部(Bu)农(Nong)产(Chan)品(Pin)质(Zhi)量(Liang)安(An)全(Quan)监(Jian)管(Guan)司(Si)提(Ti)出(Chu)。本(Ben)文(Wen)件(Jian)由(You)农(Nong)业(Ye)农(Nong)村(Cun)部(Bu)农(Nong)产(Chan)品(Pin)营(Ying)养(Yang)标(Biao)准(Zhun)专(Zhuan)家(Jia)委(Wei)员(Yuan)会(Hui)归(Gui)口(Kou)。本(Ben)文(Wen)件(Jian)起(Qi)草(Cao)单(Dan)位(Wei):北(Bei)京(Jing)工(Gong)业(Ye)大(Da)学(Xue)、浙(Zhe)江(Jiang)省(Sheng)农(Nong)业(Ye)科(Ke)学(Xue)院(Yuan)、广(Guang)西(Xi)壮(Zhuang)族(Zu)自(Zi)治(Zhi)区(Qu)农(Nong)业(Ye)科(Ke)学(Xue)院(Yuan)。本(Ben)文(Wen)件(Jian)主(Zhu)要(Yao)起(Qi)草(Cao)人(Ren):张(Zhang)芳(Fang)、齐(Qi)沛(Pei)沛(Pei)、王(Wang)颖(Ying)、王(Wang)雨(Yu)婷(Zuo)、智(Zhi)美(Mei)丽(Li)、裴(Pei)鹭(Zuo)羽(Yu)、李(Li)宜(Yi)珊(Shan)、严(Yan)华(Hua)兵(Bing)、尚(Shang)小(Xiao)红(Hong)。1范(Fan)围(Wei)本(Ben)文(Wen)件(Jian)规(Gui)定(Ding)了(Liao)葛(Ge)根(Gen)中(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)的(De)高(Gao)效(Xiao)液(Ye)相(Xiang)色(Se)谱(Pu)-串(Chuan)联(Lian)质(Zhi)谱(Pu)的(De)定(Ding)量(Liang)检(Jian)测(Ce)方(Fang)法(Fa)。本(Ben)文(Wen)件(Jian)适(Shi)用(Yong)于(Yu)野(Ye)葛(Ge)和(He)粉(Fen)葛(Ge)中(Zhong)葛(Ge)根(Gen)素(Su)、3'-羟(Zuo)基(Ji)葛(Ge)根(Gen)素(Su)、3'-甲(Jia)氧(Yang)基(Ji)葛(Ge)根(Gen)素(Su)、大(Da)豆(Dou)苷(Zuo)、大(Da)豆(Dou)苷(Zuo)元(Yuan)、染(Ran)料(Liao)木(Mu)素(Su)、染(Ran)料(Liao)木(Mu)苷(Zuo)、刺(Ci)芒(Mang)柄(Bing)花(Hua)苷(Zuo)、刺(Ci)芒(Mang)柄(Bing)花(Hua)黄(Huang)素(Su)、异(Yi)甘(Gan)草(Cao)素(Su)和(He)鹰(Ying)嘴(Zui)豆(Dou)芽(Ya)素(Su)A等(Deng)11种(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)含(Han)量(Liang)的(De)测(Ce)定(Ding)。2规(Gui)范(Fan)性(Xing)引(Yin)用(Yong)文(Wen)件(Jian)下(Xia)列(Lie)文(Wen)件(Jian)中(Zhong)的(De)内(Nei)容(Rong)通(Tong)过(Guo)文(Wen)中(Zhong)的(De)规(Gui)范(Fan)性(Xing)引(Yin)用(Yong)而(Er)构(Gou)成(Cheng)本(Ben)文(Wen)件(Jian)必(Bi)不(Bu)可(Ke)少(Shao)的(De)务(Wu)款(Kuan)。其(Qi)中(Zhong)。注(Zhu)日(Ri)期(Qi)的(De)引(Yin)用(Yong)文(Wen)件(Jian),仅(Jin)该(Gai)日(Ri)期(Qi)对(Dui)应(Ying)的(De)版(Ban)本(Ben)适(Shi)用(Yong)于(Yu)本(Ben)文(Wen)件(Jian);不(Bu)注(Zhu)日(Ri)期(Qi)的(De)引(Yin)用(Yong)文(Wen)件(Jian),其(Qi)最(Zui)新(Xin)版(Ban)本(Ben)(包(Bao)括(Kuo)所(Suo)有(You)的(De)修(Xiu)改(Gai)单(Dan))适(Shi)用(Yong)于(Yu)本(Ben)文(Wen)件(Jian)。GB/T 6682分(Fen)析(Xi)实(Shi)验(Yan)室(Shi)用(Yong)水(Shui)规(Gui)格(Ge)和(He)试(Shi)险(Xian)方(Fang)法(Fa)。3术(Shu)语(Yu)和(He)定(Ding)义(Yi)本(Ben)文(Wen)件(Jian)没(Mei)有(You)需(Xu)要(Yao)界(Jie)定(Ding)的(De)术(Shu)语(Yu)和(He)定(Ding)义(Yi)。4原(Yuan)理(Li)葛(Ge)根(Gen)样(Yang)品(Pin)中(Zhong)的(De)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)用(Yong)乙(Yi)醇(Chun)水(Shui)溶(Rong)液(Ye)超(Chao)声(Sheng)提(Ti)取(Qu),采(Cai)用(Yong)高(Gao)效(Xiao)液(Ye)相(Xiang)色(Se)谱(Pu)串(Chuan)联(Lian)质(Zhi)谱(Pu)仪(Yi)测(Ce)定(Ding),外(Wai)标(Biao)法(Fa)定(Ding)量(Liang)。5试(Shi)剂(Ji)和(He)材(Cai)料(Liao)除(Chu)非(Fei)另(Ling)有(You)规(Gui)定(Ding),所(Suo)有(You)试(Shi)剂(Ji)均(Jun)为(Wei)分(Fen)析(Xi)纯(Chun)。5.1试(Shi)剂(Ji)5.1.1水(Shui):GB/T 6682,一(Yi)级(Ji)。5.1.2甲(Jia)醇(Chun)(CH40):色(Se)谱(Pu)纯(Chun)。5.1.3甲(Jia)酸(Suan)(CH2O2):色(Se)谱(Pu)纯(Chun)。5.1.4 乙(Yi)醇(Chun)(C2H6O):分(Fen)析(Xi)纯(Chun)5.2试(Shi)剂(Ji)配(Pei)制(Zhi)5.2.1 10%甲(Jia)醇(Chun)溶(Rong)液(Ye):取(Qu)10 mL,甲(Jia)醇(Chun)(5.1.2),加(Jia)水(Shui)(5.1.1)定(Ding)容(Rong)至(Zhi)100 mL,混(Hun)匀(Yun)。5.2.2 30%乙(Yi)醇(Chun)溶(Rong)液(Ye):取(Qu)30 ml,乙(Yi)醇(Chun)(5.1. 4).加(Jia)水(Shui)(5.1.1)定(Ding)容(Rong)至(Zhi)100 mL,混(Hun)匀(Yun)。5.3标(Biao)准(Zhun)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)标(Biao)准(Zhun)品(Pin):相(Xiang)关(Guan)信(Xin)息(Xi)见(Jian)表(Biao)1,纯(Chun)度(Du)不(Bu)低(Di)于(Yu)98%。5.4标(Biao)准(Zhun)溶(Rong)液(Ye)配(Pei)制(Zhi)5.4.1黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)标(Biao)准(Zhun)储(Chu)备(Bei)液(Ye):准(Zhun)确(Que)称(Cheng)取(Qu)11种(Zhong)(表(Biao)1)待(Dai)测(Ce)物(Wu)质(Zhi)的(De)标(Biao)准(Zhun)品(Pin),用(Yong)甲(Jia)醇(Chun)(5.1.2)溶(Rong)解(Jie)后(Hou),加(Jia)入(Ru)10%甲(Jia)醇(Chun)溶(Rong)液(Ye)(5.2.1)定(Ding)量(Liang)稀(Xi)释(Shi),制(Zhi)成(Cheng)高(Gao)浓(Nong)度(Du)单(Dan)标(Biao)准(Zhun)品(Pin)储(Chu)备(Bei)液(Ye)。分(Fen)别(Bie)移(Yi)取(Qu)一(Yi)定(Ding)量(Liang)的(De)11种(Zhong)单(Dan)标(Biao)准(Zhun)品(Pin)储(Chu)备(Bei)液(Ye)于(Yu)25 mL容(Rong)量(Liang)瓶(Ping),10%甲(Jia)醇(Chun)溶(Rong)液(Ye)(5.2.1)定(Ding)容(Rong),制(Zhi)成(Cheng)10 mg/L的(De)母(Mu)液(Ye)作(Zuo)为(Wei)标(Biao)准(Zhun)品(Pin)储(Chu)备(Bei)液(Ye)。避(Bi)光(Guang)-18℃以(Yi)下(Xia)保(Bao)存(Cun),备(Bei)用(Yong)。5.4.2黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye):用(Yong)10%甲(Jia)醇(Chun)溶(Rong)液(Ye)(5.2.1)对(Dui)10 mg/L的(De)母(Mu)液(Ye)(5.4. 1)稀(Xi)释(Shi)配(Pei)成(Cheng)不(Bu)同(Tong)浓(Nong)度(Du)的(De)混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)用(Yong)于(Yu)绘(Hui)制(Zhi)标(Biao)准(Zhun)曲(Qu)线(Xian)。混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)应(Ying)现(Xian)用(Yong)现(Xian)配(Pei)。6仪(Yi)器(Qi)设(She)备(Bei)6.1超(Chao)高(Gao)效(Xiao)液(Ye)相(Xiang)色(Se)谱(Pu)-串(Chuan)联(Lian)质(Zhi)谱(Pu)仪(Yi):配(Pei)有(You)电(Dian)喷(Pen)雾(Wu)离(Li)子(Zi)源(Yuan)( ESI)。6.2电(Dian)热(Re)鼓(Gu)风(Feng)干(Gan)燥(Zao)箱(Xiang):温(Wen)度(Du)50℃~330℃,功(Gong)率(Lv)3.1 kW。6.3超(Chao)声(Sheng)波(Bo)清(Qing)洗(Xi)器(Qi):超(Chao)声(Sheng)输(Shu)入(Ru)功(Gong)率(Lv)200 W。6.4离(Li)心(Xin)机(Ji):转(Zhuan)速(Su)不(Bu)低(Di)于(Yu)7 500 r/min。6.5超(Chao)细(Xi)水(Shui)冷(Leng)式(Shi)粉(Fen)碎(Sui)机(Ji):细(Xi)度(Du)20目(Mu)~180目(Mu)(0.85mm~0.09mm),功(Gong)率(Lv)2.5kW。6.6天(Tian)平(Ping):感(Gan)量(Liang)0.001 g和(He)0.000 1 go7试(Shi)样(Yang)制(Zhi)备(Bei)7.1试(Shi)样(Yang)制(Zhi)备(Bei)新(Xin)鲜(Xian)葛(Ge)根(Gen)经(Jing)清(Qing)洗(Xi)去(Qu)掉(Diao)泥(Ni)沙(Sha)、去(Qu)皮(Pi),用(Yong)切(Qie)片(Pian)机(Ji)切(Qie)成(Cheng)2 mm薄(Bao)片(Pian)后(Hou),放(Fang)置(Zhi)于(Yu)托(Tuo)盘(Pan)中(Zhong),于(Yu)70℃烘(Hong)箱(Xiang)中(Zhong)烘(Hong)干(Gan)至(Zhi)恒(Heng)重(Zhong)。然(Ran)后(Hou)用(Yong)分(Fen)级(Ji)超(Chao)细(Xi)水(Shui)冷(Leng)式(Shi)粉(Fen)碎(Sui)机(Ji)将(Jiang)葛(Ge)根(Gen)样(Yang)品(Pin)粉(Fen)碎(Sui),全(Quan)部(Bu)装(Zhuang)入(Ru)洁(Jie)净(Jing)的(De)容(Rong)器(Qi)中(Zhong),立(Li)即(Ji)检(Jian)测(Ce)。如(Ru)果(Guo)需(Xu)要(Yao)较(Jiao)长(Chang)时(Shi)间(Jian)保(Bao)存(Cun),将(Jiang)样(Yang)品(Pin)密(Mi)封(Feng)、标(Biao)记(Ji)后(Hou)于(Yu)-18℃以(Yi)下(Xia)保(Bao)存(Cun)。7.2 试(Shi)样(Yang)提(Ti)取(Qu)称(Cheng)取(Qu)葛(Ge)根(Gen)粉(Fen)末(Mo)0.5 g(精(Jing)确(Que)至(Zhi)0.000 1 g),置(Zhi)于(Yu)50 mL离(Li)心(Xin)管(Guan)中(Zhong),加(Jia)入(Ru)25 ml 30%乙(Yi)醇(Chun)溶(Rong)液(Ye)(5.2.2),室(Shi)温(Wen)下(Xia)超(Chao)声(Sheng)提(Ti)取(Qu)45 min。于(Yu)7 500 r/min离(Li)心(Xin)5 min,将(Jiang)上(Shang)清(Qing)液(Ye)转(Zhuan)移(Yi)至(Zhi)50 mL容(Rong)量(Liang)瓶(Ping)中(Zhong)。沉(Chen)淀(Dian)物(Wu)再(Zai)用(Yong)30%乙(Yi)醇(Chun)溶(Rong)液(Ye)(5.2. 2)洗(Xi)涤(Di)2次(Ci),每(Mei)次(Ci)用(Yong)量(Liang)约(Yue)5 mL。在(Zai)相(Xiang)同(Tong)条(Tiao)件(Jian)下(Xia)离(Li)心(Xin)5 min,合(He)并(Bing)上(Shang)清(Qing)液(Ye), 30%乙(Yi)醇(Chun)溶(Rong)液(Ye)(5.2.2)定(Ding)容(Rong)至(Zhi)50 mL。上(Shang)样(Yang)前(Qian),采(Cai)用(Yong)0.22μm有(You)机(Ji)相(Xiang)滤(Lv)膜(Mo)过(Guo)滤(Lv)(5.5)。8测(Ce)定(Ding)8.1超(Chao)高(Gao)效(Xiao)液(Ye)相(Xiang)色(Se)谱(Pu)参(Can)考(Kao)条(Tiao)件(Jian)8.1.1色(Se)谱(Pu)柱(Zhu):ACE Excel C18柱(Zhu)(100mm×2.1mm×1.7μm)或(Huo)性(Xing)能(Neng)相(Xiang)当(Dang)者(Zhe)。8.1.2流(Liu)动(Dong)相(Xiang) A:甲(Jia)醇(Chun)(5.1.2)。8.1.3流(Liu)动(Dong)相(Xiang) B:0. 1%甲(Jia)酸(Suan)水(Shui)溶(Rong)液(Ye),取(Qu)0.1 mL甲(Jia)酸(Suan)(5.1. 3)加(Jia)水(Shui)(5.1.1)定(Ding)容(Rong)至(Zhi)100 mL,混(Hun)匀(Yun)。8.1.4柱(Zhu)温(Wen):40℃。8. 1.5 流(Liu)速(Su):0.3 mL/min。8.1.6进(Jin)样(Yang)量(Liang) :10μL。8.1.7流(Liu)动(Dong)相(Xiang):梯(Ti)度(Du)洗(Xi)脱(Tuo)程(Cheng)序(Xu)见(Jian)表(Biao)2。8.2质(Zhi)谱(Pu)参(Can)考(Kao)条(Tiao)件(Jian)8.2.1扫(Sao)描(Miao)方(Fang)式(Shi):正(Zheng)负(Fu)离(Li)子(Zi)扫(Sao)描(Miao)。8.2.2离(Li)子(Zi)化(Hua)电(Dian)压(Ya):4 000 V。8.2.3毛(Mao)细(Xi)管(Guan)温(Wen)度(Du):250℃。8.2.4碰(Peng)撞(Zhuang)气(Qi)体(Ti):氩(Zuo)气(Qi)(纯(Chun)度(Du)为(Wei)99. 99%),压(Ya)力(Li)为(Wei)270 kPa。8.2.5雾(Wu)化(Hua)气(Qi):氮(Dan)气(Qi)(纯(Chun)度(Du)为(Wei)97%以(Yi)上(Shang)),流(Liu)速(Su)为(Wei)3. 0 L/min。8.2.6辅(Fu)助(Zhu)气(Qi):氮(Dan)气(Qi)(纯(Chun)度(Du)为(Wei)97%以(Yi)上(Shang)) ,流(Liu)速(Su)为(Wei)10.0 L/min。8.2.7检(Jian)测(Ce)方(Fang)式(Shi): 多(Duo)反(Fan)应(Ying)监(Jian)测(Ce)(MRM)。8.2.8黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)保(Bao)留(Liu)时(Shi)间(Jian)和(He)监(Jian)测(Ce)离(Li)子(Zi)对(Dui)信(Xin)息(Xi)见(Jian)附(Fu)录(Lu)A.3.3 供(Gong)试(Shi)样(Yang)品(Pin)的(De)测(Ce)定(Ding)在(Zai)仪(Yi)器(Qi)的(De)最(Zui)佳(Jia)条(Tiao)件(Jian)下(Xia),分(Fen)别(Bie)取(Qu)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)(5.4.2)与(Yu)葛(Ge)根(Gen)素(Su)等(Deng)11种(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)样(Yang)品(Pin)(7.2)上(Shang)机(Ji)测(Ce)定(Ding)。混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)中(Zhong)11种(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)总(Zong)离(Li)子(Zi)色(Se)谱(Pu)图(Tu)和(He)各(Ge)组(Zu)分(Fen)离(Li)子(Zi)色(Se)谱(Pu)图(Tu)见(Jian)附(Fu)录(Lu)A。8.4定(Ding)性(Xing)测(Ce)量(Liang)在(Zai)相(Xiang)同(Tong)试(Shi)验(Yan)条(Tiao)件(Jian)下(Xia)测(Ce)定(Ding)试(Shi)样(Yang)和(He)混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye),若(Ruo)样(Yang)品(Pin)溶(Rong)液(Ye)中(Zhong)检(Jian)出(Chu)色(Se)谱(Pu)峰(Feng)的(De)保(Bao)留(Liu)时(Shi)间(Jian)与(Yu)基(Ji)质(Zhi)标(Biao)准(Zhun)溶(Rong)液(Ye)中(Zhong)目(Mu)标(Biao)物(Wu)色(Se)谱(Pu)峰(Feng)的(De)保(Bao)留(Liu)时(Shi)间(Jian)一(Yi)致(Zhi)(变(Bian)化(Hua)范(Fan)围(Wei)在(Zai)±2.5%),且(Qie)样(Yang)品(Pin)溶(Rong)液(Ye)的(De)质(Zhi)谱(Pu)离(Li)子(Zi)对(Dui)相(Xiang)对(Dui)丰(Feng)度(Du)与(Yu)依(Yi)度(Du)相(Xiang)当(Dang)基(Ji)质(Zhi)标(Biao)准(Zhun)溶(Rong)液(Ye)的(De)质(Zhi)谱(Pu)离(Li)子(Zi)对(Dui)相(Xiang)对(Dui)丰(Feng)度(Du)相(Xiang)比(Bi)较(Jiao),相(Xiang)对(Dui)离(Li)子(Zi)丰(Feng)度(Du)的(De)相(Xiang)对(Dui)偏(Pian)差(Cha)不(Bu)超(Chao)过(Guo)表(Biao)3规(Gui)定(Ding)的(De)范(Fan)围(Wei),则(Ze)可(Ke)判(Pan)定(Ding)样(Yang)品(Pin)中(Zhong)存(Cun)在(Zai)该(Gai)组(Zu)分(Fen)。混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)中(Zhong)各(Ge)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)离(Li)子(Zi)色(Se)谱(Pu)图(Tu)见(Jian)附(Fu)录(Lu)B。8.5定(Ding)量(Liang)测(Ce)量(Liang)以(Yi)不(Bu)同(Tong)浓(Nong)度(Du)混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)的(De)浓(Nong)度(Du)为(Wei)横(Heng)坐(Zuo)标(Biao),色(Se)谱(Pu)峰(Feng)面(Mian)积(Ji)(响(Xiang)应(Ying)值(Zhi))为(Wei)纵(Zong)坐(Zuo)标(Biao),绘(Hui)制(Zhi)标(Biao)准(Zhun)曲(Qu)线(Xian),标(Biao)准(Zhun)曲(Qu)线(Xian)的(De)相(Xiang)关(Guan)系(Xi)数(Shu)应(Ying)不(Bu)低(Di)于(Yu)0.99。试(Shi)样(Yang)溶(Rong)液(Ye)与(Yu)标(Biao)准(Zhun)溶(Rong)液(Ye)中(Zhong)待(Dai)测(Ce)物(Wu)的(De)响(Xiang)应(Ying)值(Zhi)均(Jun)应(Ying)在(Zai)仪(Yi)器(Qi)检(Jian)测(Ce)的(De)线(Xian)性(Xing)范(Fan)围(Wei)内(Nei)。如(Ru)超(Chao)出(Chu)线(Xian)性(Xing)范(Fan)围(Wei),应(Ying)重(Zhong)新(Xin)试(Shi)验(Yan)或(Huo)将(Jiang)试(Shi)样(Yang)溶(Rong)液(Ye)和(He)基(Ji)质(Zhi)匹(Pi)配(Pei)混(Hun)合(He)标(Biao)准(Zhun)系(Xi)列(Lie)溶(Rong)液(Ye)作(Zuo)相(Xiang)应(Ying)稀(Xi)释(Shi)后(Hou)重(Zhong)新(Xin)测(Ce)定(Ding)。单(Dan)点(Dian)校(Xiao)准(Zhun)定(Ding)量(Liang)时(Shi),试(Shi)样(Yang)溶(Rong)液(Ye)中(Zhong)待(Dai)测(Ce)物(Wu)的(De)浓(Nong)度(Du)与(Yu)溶(Rong)剂(Ji)混(Hun)合(He)标(Biao)准(Zhun)溶(Rong)液(Ye)的(De)浓(Nong)度(Du)相(Xiang)差(Cha)不(Bu)超(Chao)过(Guo)30%。标(Biao)准(Zhun)加(Jia)入(Ru)法(Fa)则(Ze)以(Yi)添(Tian)加(Jia)的(De)标(Biao)准(Zhun)溶(Rong)液(Ye)浓(Nong)度(Du)为(Wei)横(Heng)坐(Zuo)标(Biao)、色(Se)谱(Pu)峰(Feng)面(Mian)积(Ji)(响(Xiang)应(Ying)值(Zhi))为(Wei)纵(Zong)坐(Zuo)标(Biao),绘(Hui)制(Zhi)标(Biao)准(Zhun)曲(Qu)线(Xian),并(Bing)外(Wai)推(Tui)至(Zhi)浓(Nong)度(Du)坐(Zuo)标(Biao)轴(Zhou)。8.6结(Jie)果(Guo)计(Ji)算(Suan)用(Yong)液(Ye)相(Xiang)色(Se)谱(Pu)质(Zhi)谱(Pu)数(Shu)据(Ju)处(Chu)理(Li)软(Ruan)件(Jian)或(Huo)者(Zhe)按(An)照(Zhao)公(Gong)式(Shi)计(Ji)算(Suan)试(Shi)样(Yang)中(Zhong)检(Jian)测(Ce)目(Mu)标(Biao)物(Wu)量(Liang),按(An)公(Gong)式(Shi)(1)计(Ji)算(Suan)。式(Shi)中(Zhong):ω——试(Shi)样(Yang)中(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)的(De)含(Han)量(Liang)的(De)数(Shu)值(Zhi),单(Dan)位(Wei)为(Wei)毫(Hao)克(Ke)每(Mei)千(Qian)克(Ke)(mg/kg);A——样(Yang)品(Pin)中(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)的(De)峰(Feng)面(Mian)积(Ji);ρS——标(Biao)准(Zhun)溶(Rong)液(Ye)浓(Nong)度(Du) 的(De)数(Shu)值(Zhi),单(Dan)位(Wei)为(Wei)毫(Hao)克(Ke)每(Mei)升(Sheng)(mg/L);V——定(Ding)容(Rong)体(Ti)积(Ji)的(De)数(Shu)值(Zhi), 单(Dan)位(Wei)为(Wei)毫(Hao)升(Sheng)(mL);f——稀(Xi)释(Shi)倍(Bei)数(Shu);AS——标(Biao)样(Yang)中(Zhong)黄(Huang)酮(Tong)类(Lei)化(Hua)合(He)物(Wu)的(De)峰(Feng)面(Mian)积(Ji);m——最(Zui)终(Zhong)溶(Rong)液(Ye)所(Suo)代(Dai)表(Biao)的(De)试(Shi)样(Yang)质(Zhi)量(Liang)的(De)数(Shu)值(Zhi),单(Dan)位(Wei)为(Wei)克(Ke)(g)。注(Zhu):计(Ji)算(Suan)结(Jie)果(Guo)应(Ying)扣(Kou)除(Chu)空(Kong)白(Bai)值(Zhi),测(Ce)定(Ding)结(Jie)果(Guo)用(Yong)平(Ping)行(Xing)测(Ce)定(Ding)的(De)算(Suan)术(Shu)平(Ping)均(Jun)值(Zhi)表(Biao)示(Shi),保(Bao)留(Liu)3位(Wei)有(You)效(Xiao)数(Shu)字(Zi)。9精(Jing)密(Mi)度(Du)9.1 重(Zhong)复(Fu)性(Xing)在(Zai)重(Zhong)复(Fu)性(Xing)条(Tiao)件(Jian)下(Xia)获(Huo)得(De)的(De)2次(Ci)独(Du)立(Li)的(De)测(Ce)定(Ding)结(Jie)果(Guo)的(De)绝(Jue)对(Dui)差(Cha)值(Zhi)不(Bu)大(Da)于(Yu)这(Zhe)2个(Ge)测(Ce)定(Ding)值(Zhi)的(De)算(Suan)术(Shu)平(Ping)均(Jun)值(Zhi)的(De)15%。9.2 再(Zai)现(Xian)性(Xing)在(Zai)再(Zai)现(Xian)性(Xing)条(Tiao)件(Jian)下(Xia)获(Huo)得(De)的(De)2次(Ci)独(Du)立(Li)的(De)测(Ce)定(Ding)结(Jie)果(Guo)的(De)绝(Jue)对(Dui)差(Cha)值(Zhi)大(Da)于(Yu)2个(Ge)测(Ce)定(Ding)值(Zhi)的(De)算(Suan)术(Shu)平(Ping)均(Jun)值(Zhi)的(De)15%。10检(Jian)出(Chu)限(Xian)和(He)定(Ding)量(Liang)限(Xian)葛(Ge)根(Gen)样(Yang)品(Pin)中(Zhong)大(Da)豆(Dou)苷(Zuo)、葛(Ge)根(Gen)素(Su)、3'-甲(Jia)氧(Yang)基(Ji)葛(Ge)根(Gen)素(Su)和(He)刺(Ci)芒(Mang)柄(Bing)花(Hua)黄(Huang)素(Su)的(De)检(Jian)出(Chu)限(Xian)为(Wei)0.01 mg/kg, 定(Ding)量(Liang)限(Xian)为(Wei)0.03 mg/kg;刺(Ci)芒(Mang)柄(Bing)花(Hua)苷(Zuo)、3'-甲(Jia)氧(Yang)基(Ji)葛(Ge)根(Gen)素(Su)和(He)异(Yi)甘(Gan)草(Cao)素(Su)的(De)检(Jian)出(Chu)最(Zui)为(Wei)0.02mg/kg,定(Ding)量(Liang)限(Xian)为(Wei)0.07 mg/kg;大(Da)豆(Dou)苷(Zuo)元(Yuan)、染(Ran)料(Liao)木(Mu)素(Su)、染(Ran)料(Liao)木(Mu)苷(Zuo)和(He)鹰(Ying)嘴(Zui)豆(Dou)芽(Ya)素(Su)A的(De)检(Jian)出(Chu)限(Xian)为(Wei)0.03mg/kg,定(Ding)量(Liang)限(Xian)为(Wei)0.1 mg/kg。转(Zhuan)载(Zai)自(Zi):http://www.xpl-hplc.com/enstyle/articleinfo_11801576.html
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