一(yi)、CMC配制：CMC的濃度為3-4‰。在500ml燒杯中加(jia)入150ml水，在磁力攪(jiao)拌器攪(jiao)拌下慢慢加(jia)入1.75gCMC，促使(shi)其溶(rong)(rong)解，攪(jiao)拌20min后，再加(jia)入350ml水，一(yi)直攪(jiao)拌1h。抽濾得(de)CMC溶(rong)(rong)液待用。

二、硅(gui)(gui)膠(jiao)(jiao)液配制：在研(yan)(yan)缽中加入(ru)約(yue)100ml上(shang)述(shu)CMC溶液，用研(yan)(yan)棒(bang)不斷攪拌下，慢(man)慢(man)加入(ru)硅(gui)(gui)膠(jiao)(jiao)GF254粉末（CMC水溶液的(de)用量大約(yue)是硅(gui)(gui)膠(jiao)(jiao)質(zhi)量的(de)2-3倍之間），直(zhi)至感(gan)到液體變得較粘(zhan)稠狀，且(qie)用研(yan)(yan)棒(bang)蘸取硅(gui)(gui)膠(jiao)(jiao)液可見(jian)粘(zhan)絲狀即(ji)可。切記不能(neng)馬上(shang)就開(kai)始鋪(pu)板(ban)，需要(yao)將其再放置(zhi)約(yue)十幾分(fen)(fen)鐘，以使硅(gui)(gui)膠(jiao)(jiao)粉末能(neng)夠充分(fen)(fen)吸收水分(fen)(fen)溶脹，過早鋪(pu)板(ban)，將會造成(cheng)硅(gui)(gui)膠(jiao)(jiao)板(ban)起(qi)泡(pao)、起(qi)鼓或起(qi)楞等(deng)。

三、鋪板(ban)(ban)：用藥勺取適(shi)量硅膠(jiao)液置于玻(bo)璃板(ban)(ban)上(shang)，并用藥勺大致均勻地攤開，尤其四個角及邊緣鋪滿，然后將該(gai)玻(bo)璃板(ban)(ban)在(zai)桌面上(shang)做上(shang)下地且幅(fu)度要(yao)大些顛(dian)動幾次即(ji)可。

四、干(gan)燥：自(zi)然晾干(gan)十幾小時。

五、活化：放(fang)在(zai)恒溫(wen)(wen)干(gan)燥(zao)(zao)箱里于105-110℃干(gan)燥(zao)(zao)30min，然后冷卻(que)室溫(wen)(wen)，取出存放(fang)在(zai)干(gan)燥(zao)(zao)器保存，待用(yong)。

薄層色(se)譜點(dian)樣應(ying)注意的(de)問題：

1.點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)量：原點(dian)(dian)(dian)(dian)位置對樣(yang)(yang)(yang)品(pin)容積的負(fu)荷量有限，體積不宜(yi)太大，一般為?0.5~10μl，樣(yang)(yang)(yang)品(pin)的濃(nong)度通(tong)常為0.5~2mg，太濃(nong)時展開(kai)(kai)劑(ji)從原點(dian)(dian)(dian)(dian)外圍繞(rao)行而(er)不是通(tong)過整個原點(dian)(dian)(dian)(dian)把它帶動向前，使斑點(dian)(dian)(dian)(dian)脫(tuo)尾(wei)或(huo)重疊，降低(di)分離效率(lv)。點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)量太小，不能檢出清晰的斑點(dian)(dian)(dian)(dian)影響判斷。點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)量太多，展開(kai)(kai)劑(ji)不能全部負(fu)載(zai)，容易產生脫(tuo)尾(wei)現(xian)象(xiang)。當點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)量適合時，可(ke)(ke)采用點(dian)(dian)(dian)(dian)狀點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)；當點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)量過大，原點(dian)(dian)(dian)(dian)無法負(fu)荷時，可(ke)(ke)采用條帶狀點(dian)(dian)(dian)(dian)樣(yang)(yang)(yang)，得到更(geng)好(hao)的分離效果，提高分辨率(lv)。

2.樣(yang)品(pin)的(de)(de)溶劑(ji)：樣(yang)品(pin)在(zai)溶劑(ji)中(zhong)(zhong)溶解(jie)度很(hen)大(da)，原(yuan)點(dian)將變成空心圓，影響(xiang)隨后的(de)(de)線性(xing)展(zhan)開，所以原(yuan)則上(shang)應選擇對(dui)被(bei)測成分(fen)可以溶解(jie)但溶解(jie)度不(bu)(bu)是(shi)很(hen)大(da)的(de)(de)溶劑(ji)。供試液的(de)(de)溶劑(ji)在(zai)原(yuan)點(dian)殘留會改變展(zhan)開的(de)(de)選擇性(xing)，親(qin)水性(xing)溶劑(ji)殘留在(zai)原(yuan)點(dian)吸(xi)收大(da)氣中(zhong)(zhong)的(de)(de)水分(fen)(特別在(zai)高(gao)(gao)濕度環境)對(dui)色譜(pu)質量也會產生影響(xiang)，因(yin)此除去原(yuan)點(dian)殘存溶劑(ji)是(shi)必(bi)要的(de)(de)，但對(dui)遇熱(re)(re)不(bu)(bu)穩定(ding)和易揮發的(de)(de)成分(fen)，應避免高(gao)(gao)溫加熱(re)(re)，以免成分(fen)被(bei)破壞或(huo)損失。