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干货丨合成着色剂分析之赤藓红分析回收率不稳定?安谱实验带你揭秘真相!
发布时间:2020-11-23   点击次数:87次

之前我们曾探讨过亮蓝分析有杂峰干扰的原因靛蓝分析回收率不稳定的原因,亮蓝分析有杂峰干扰是因为亮蓝存在3个同分异构体,靛蓝回收率不稳定是因为温度、光照、时间等因素会影响靛蓝溶液的稳定性。

GUANYUHECHENGZHESEJIDEFENXIWOMENYOUYIXILIEDEXIAOZHISHIXIANGHEDAJIAFENXIANG,JINTIANWEIDAJIADAILAIDESHIGUANYUCHIXIANHONGFENXISHIHUISHOULVBUWENDINGDEYUANYIN。

BENWENSUOZHIDECHIXIANHONG,CASSHI16423-68-0,WOMENCHENGZHIWEICHIXIANHONGSHICANKAO《GB 5009.35-2016 SHIPINANQUANguoJIABIAOZHUN SHIPINZHONGHECHENGZHESEJIDECEDING》,ZAIMOUXIEWENXIANZILIAOZHONGDAJIAKENENGHUIKANDAOJIANGCASSHI16423-68-0DEWUZHICHENGZHIWEICHIXIANHONGB,ZHUYAOYOUYUSUCHENGDEWENTI。WANGSHANGSOUSUOCHIXIANHONG,NIYIDINGHUISOUSUODAOLIANGGEBUTONGCASDEHUAHEWU,HAIYOUYIGECASHAOSHI568-63-8,TONGGUOBIJIAOHUAXUESHI,KEYIKANCHUZHEILIANGGEHUAHEWUHUWEITONGFENYIGOUTI。CASHAOSHIHUAHEWUDESHENfenZHENG,SHIHUAHEWUDEWEIyiBIAOSHI,ZAIHECHENGZHESEJIFENXISHISHOUSUCHENGDEYINGXIANG,HENRONGYIXUANCUOFENXIDUIXIANG,JIANYIDAJIAZAIXUANGOUHECHENGZHESEJIDESHIHOU,YIDINGYAOJIANGCASHAOZUOWEIWEIyiBIAOSHI。

image.png

CAS:16423-68-0 

image.png

CAS:568-63-8

ZAIGB 5009.35ZHONGYOUYIZHONGHECHENGZHESEJIDETIQUFANGFA:JUXIANANXIFUFA。ZAICAOZUODESHIHOUHENBUFANGBIAN,MUQIANYIJINGYOUSHANGPINHUADEJUXIANANGUXIANGCUIQUXIAOZHUDAITI,BIRUANPUSHIYANDECNW Poly-sery PA JUXIANANXIAOZHU,YINQICAOZUOFANGBIAN、JIESHENGSHIJIAN、JIESHENGSHIJI、DUIDUOZHONGHECHENGZHESEJICHULIHOUJIEGUOZHUNQUEQIEHUISHOULVGAO,YINERBEISHOUGUANGDAXIAOFEIZHEDEQINGLAI,JIANGQIYONGYU8ZHONGHECHENGZHESEJIDEQIANCHULISHIYANGUOCHENGHEJIEGUORUXIAWENSUOSHI。

SPE

XIAOZHU:CNW Poly-sery PA JUXIANANXIAOZHU  (500mg/6mL)

HUOHUA:5mLJIACHUN

PINGHENG:5mL SHUI

SHANGYANG:5mL 1ppm 8ZHONGHECHENGZHESEJIBIAOZHUNPIN,RONGJININGMENGSUANRONGYE(pH 3.0~4.0)

LINXI:5mL JIACHUN:JIASUAN:QULIZISHUI(4:2:4)(V/V/V),LINXIHOUCHOUGANXIAOZHUZHONGDERONGYE

XITUO:3mL*2 10%ANSHUIJIACHUN

SHOUJIXITUOYE,BINGYU50℃DANCHUIZHIGAN,YONGJIACHUN:0.02MYISUANANRONGYE(1:1)DINGRONGZHI1mL,CHONGFENRONGJIEHOU,SHANGJIFENXI。

仪器条件

SEPUZHU: C18-Wp(4.6mm*250mm,5um)

LIUDONGXIANG:A:JIACHUNB:0.02MYISUANAN

TIDUXITUO:0min 15%A,5min 35% A,12~22min 95%A,22.5~30min 15 %A

LIUSU:1.0mL/min

ZHUWEN:25℃

BOZHANG:254nm

JINYANGLIANG:10ul

实验结果

BIAO1 8ZHONGHECHENGZHESEJISHIYANJIEGUO

image.png

JIEGUOBIAOMING,CHUCHIXIANHONGZHIWAI,QITA7ZHONGHECHENGZHESEJIDEHUISHOULVJUNDAYU90%,RSDXIAOYU5%,WEIDUCHIXIANHONGHUISHOULVJIAODI,QIEDUOCISHIYANFAXIANQIHUISHOULVZAI70%~90%ZHIJIAN,HUISHOULVBUWENDING。

原因分析

NEIMEDAODISHISHENMEYUANYINDAOZHICHIXIANHONGHUISHOULVBUWENDINGNI。ZIXIYUEDUGUOBIAO,KEYIFAXIANDUIYUHANCHIXIANHONGDEYANGPIN,QITIQUFANGFACAIYONGDESHIYEYE——FENPEIFA,ERFEIJUXIANANXIFUFA,DANSHIGUOBIAOBINGMEIYOUDUICHIXIANHONGWEIHEBUNENGCAIYONGJUXIANANXIFUFAZUOJIESHISHUOMING。JIEHECHIXIANHONGDEHUAXUEJIEGOUHEGB 5009.35WOMENLAIFENXIYIXIAYUANYIN。

YE-YEFENPEIFAYUANLI,JIAYANSUANSHICHIXIANHONGJIEGOUSHANGDENaFANYINGHOUBIANWEIH,CHIXIANHONGFENZISHANGDEFENQIANGJIYUSANZHENGXINANFENZIZHONGDEDANYUANZIXINGCHENGQINGJIAN,SHENGCHENGBURONGYUSHUIDEHUAHEWU,BEICUIQUDAOZHENGDINGCHUNZHONG,JIABAOHELIUSUANNAQUCHUYOUJIXIANGZHONGCANLIUDESHUIFEN,ZHENGJIWANQUCHUYOUZHILEIZAZHI,YONGANSHUIZUOFANCUIRONGJI,JIARUANSHUI,SHIHUAHEWUDEQINGJIANDUANLIE,CHIXIANHONGJINRUSHUIXIANG,YISUANDIAOpHZHIZHONGXING,NONGSUOHOUDAICE。

JUXIANANXIFUFADEYUANLI,JUXIANANSHIYOUXIANANJIANJUHEXINGCHENGDEGAOFENZIHUAHEWU,QIXIANANJIKEYUQIANGJIFENLEI、SUANLEI、KUNLEI、XIAOJIDENGHUAHEWUYIQINGJIANXINGSHIJIEHEERBEIXIFU。QITA7ZHONGHECHENGZHESEJIJUNHANYOUJIAODUODEHUANGSUANNAJITUAN,ZAISUANXINGTIAOJIANXIAZHUANBIANCHENGHUANGSUANGEN,YUJUXIANANDEJIEHEHENJINMI,JIACHUN-JIASUANRONGYEBINGBUNENGSHIQIFENLI,KEYIZUOWEILINXIRONGJI,LINXIDIAOYIXIEZAZHI,JIASHUIYEBUNENGJIANGQIFENLI,TONGSHIKEYIXIQUYIXIESHUIRONGXINGZAZHI,JIARUYICHUN-ANSHUI-SHUI,JIANGHECHENGZHESEJIJIEXICHULAI,YISUANDIAOpHZHIZHONGXING,NONGSUOHOUDAICE。SPEDEFANGFAYESHILIYONGLECIYUANLI,SUANXINGTIAOJIANSHANGYANG,SHIMUBIAOWUYUJUXIANANJIEHE,ZAIYONGYIDINGBILIDEJIACHUN:JIASUAN:QULIZISHUILINXIQUCHUZAZHI,RANHOUYONGANSHUIJIACHUNXITUODIAOMUBIAOWU,NONGSUOFURONGDAICE。SUOYIZHEI7ZHONGHECHENGZHESEJIYONGJUXIANANFENHEJUXIANANXIAOZHUJUNNENGDEDAOJIAOHAODEJIEGUO。ERCHIXIANHONGZAISUANXINGTIAOJIANXIANaFANYINGHOUBIANWEIH,FENQIANGJIYENENGYUJUXIANANJIEHEERBEIXIFU,DANSHIZAIJIACHUNYOUJIXIANGCUNZAIDETIAOJIANXIA,HEJUXIANANDEJIEHEBINGBUJINMI,RONGYIRONGJIEZAIJIACHUNZHONGSUIZHELINXIYELIUCHU,DAOZHIXITUOHUISHOULVDIQIEBUWENDING。TONGGUOSHEJILINXIHEBULINXIBUZHOUJINXINGJIEGUOBIJIAO,FAXIANBULINXISHICHIXIANHONGDEHUISHOULVDAYUE93%,MINGXIANGAOYULINXISHICHIXIANHONGDEHUISHOULV80%ZUOYOU。YINJUXIANANZAIYONGYUHECHENGZHESEJICEDINGSHILINXIKEYICHUDIAOYIXIEGANRAOFENXIDEZAZHICHENGFEN,GULINXIBUZHOUHENYOUBIYAO,RUGUOCHIXIANHONGHEQITAHECHENGZHESEJITONGSHIYONGJUXIANANXIAOZHUFENXISHI,XUYAOGUANZHULINXIRONGYEHEJIZHIDEFUZACHENGDU,JUEDINGSHIFOUXUYAOZAILINXIYEZHONGJIARUJIACHUNYOUJISHIJI。

CHULEYONGJUXIANANXIAOZHUCEDINGCHIXIANHONGSHILINXIRONGYEBUNENGYONGJIASUAN-JIACHUNRONGYEWAI,YAOSHICHIXIANHONGDESHIYANJIEGUOZHUNQUE、HUISHOULVGAOHAIXUYAOZHUYILINGWAILIANGGEFANGMIANDEWENTI:

(1)SHANGJIZHIQIANGUOLVSUOYONGDELVMOBUDESHIYONGNILONGLVMO,YINWEINILONGDEHUAXUECHENGFENJIUSHIJUXIANAN,HUIXIFUHECHENGZHESEJI;

(2)JIANYICHIXIANHONGSHANGJIRONGYEDERONGJIZHONGJIARUYIDINGBILIDEJIACHUN,RUJIACHUN:SHUI(1:1)HUOJIACHUN:0.02MYISUANAN(1:1),ERFEIYONGCHUNSHUIZUORONGJI。YINWEIWOMENDUOCISHIYANFAXIANJINGGUODANCHUINONGSUOHOU,CHUNSHUIFURONG,GUANBISHANGHUICANLIUHENDUOROUYANKEJIANDECHIXIANHONG(HONGSE),JINGGUOZHANGSHIJIANDECHAOSHENG、WOXUANDOUHENNANRONGJIEDIAO,SHANGJIFENXIHUISHOULVDAYUECAI20%ZUOYOU,DANJIARUYIDINGBILIDEJIACHUNHOUHENRONGYIJIANGCHIXIANHONGRONGJIEXIALAI,QIEJIACHUNBENLAIYESHILIUDONGXIANGDEYIBUFEN,YONGLIUDONGXIANGZUORONGJIHEQINGHELI。

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