 |
 |
 |
 |
 |
 |
||
 |
 |
 |
 |
 |
| 4 | 1/1 | 返回列表 |
| 查看: 1513 | 回復(fù): 3 | |||
yangxicshe鐵蟲 (小有名氣)
|
[交流]
【求助】溶劑峰和藥峰總是重疊在一起了，應(yīng)該怎么調(diào)整比例？ 已有3人參與
|
|
流動(dòng)相的最佳比例 各位資深人士，我是HPLC的新手，現(xiàn)在在做多西環(huán)素的HPLC的測(cè)定，在365nm的波長(zhǎng)下，流動(dòng)相是0.01M草酸-乙腈-甲醇，原來的比例是 50:35:15，但是溶劑峰和藥峰總是重疊在一起了，應(yīng)該怎么調(diào)整比例�。考状�，乙腈的吸收波長(zhǎng)又是多少呢？期盼回復(fù)！ |
回復(fù)此樓» 猜你喜歡
本人考085602 化學(xué)工程 專碩
已經(jīng)有23人回復(fù)
-
求調(diào)劑院校信息
已經(jīng)有4人回復(fù)
-
085600材料與化工306
已經(jīng)有4人回復(fù)
-
286求調(diào)劑
已經(jīng)有10人回復(fù)
-
328求調(diào)劑，英語(yǔ)六級(jí)551，有科研經(jīng)歷
已經(jīng)有9人回復(fù)
-
一志愿北京化工大學(xué)070300 學(xué)碩336求調(diào)劑
已經(jīng)有4人回復(fù)
-
286分人工智能專業(yè)請(qǐng)求調(diào)劑愿意跨考！
已經(jīng)有8人回復(fù)
-
資源與環(huán)境 調(diào)劑申請(qǐng)(333分)
已經(jīng)有5人回復(fù)
-
280求調(diào)劑
已經(jīng)有12人回復(fù)
-
269專碩求調(diào)劑
已經(jīng)有5人回復(fù)
» 本主題相關(guān)價(jià)值貼推薦，對(duì)您同樣有幫助:
- 求助：100%甲醇做流動(dòng)相，出峰仍然很晚；樣品溶劑不一樣，出峰時(shí)間也不一樣？
已經(jīng)有24人回復(fù)
- 求助：誰(shuí)有常見的氘代溶劑氫譜和碳譜化學(xué)位移數(shù)據(jù)和峰裂距，謝謝！
已經(jīng)有7人回復(fù)
- agilent GC 自動(dòng)進(jìn)樣純?nèi)軇�，主峰前總是有個(gè)很高的峰
已經(jīng)有8人回復(fù)
- 氣相色譜檢測(cè)兩物質(zhì)出峰有點(diǎn)重疊，怎么調(diào)整呢？
已經(jīng)有4人回復(fù)
- 溶劑峰與標(biāo)品峰重合怎么辦？
已經(jīng)有3人回復(fù)
- HPLC 最前面出的溶劑峰接到里面會(huì)影響核磁打譜嗎？
已經(jīng)有6人回復(fù)
- 這個(gè)大峰是溶劑峰嗎，為什么會(huì)這么的大？請(qǐng)教大家！
已經(jīng)有9人回復(fù)
- 【求助】我做氣相色譜卻總是只有溶劑峰，看不到樣品峰，求交流%>_<%
已經(jīng)有12人回復(fù)
- 【求助】HPLC兩分鐘左右出峰一定是溶劑峰嗎？
已經(jīng)有13人回復(fù)
- 【求助】做微球釋放時(shí)，總是掃描不出藥物吸收峰怎么回事？
已經(jīng)有8人回復(fù)
- 【求助】液相分析物和溶劑峰重疊了，怎么辦？
已經(jīng)有17人回復(fù)
dingjinglvde
木蟲 (正式寫手)
- 應(yīng)助: 41 (小學(xué)生)
- 金幣: 4351.6
- 紅花: 4
- 帖子: 734
- 在線: 653.7小時(shí)
- 蟲號(hào): 411754
- 注冊(cè): 2007-06-24
- 性別: GG
- 專業(yè): 藥學(xué)
★ ★
小木蟲(金幣+0.5):給個(gè)紅包，謝謝回帖交流
karl2100(金幣+1): 多謝提供！ 2011-03-11 19:48:21
小木蟲(金幣+0.5):給個(gè)紅包，謝謝回帖交流
karl2100(金幣+1): 多謝提供！ 2011-03-11 19:48:21
|
溶劑如果是流動(dòng)相，在365nm應(yīng)該沒有吸收啊 如果有峰，應(yīng)該很小，出峰時(shí)間也應(yīng)該很早的 USP33 ASSAY • Procedure Mobile phase: Transfer 2.72 g of monobasic potassium phosphate, 0.74 g of sodium hydroxide, 0.50 g of tetrabutylammonium hydrogen sulfate, and 0.40 g of edetate disodium to a 1000-mL volumetric flask. Add 850 mL of water, and stir to dissolve. Add 60 g of tertiary butyl alcohol with the aid of water, dilute with water to volume, and adjust with 1 N sodium hydroxide to a pH of 8.0 ± 0.1. Pass this solution through a filter having a porosity of 0.5 µm or finer, and degas before using. Decreasing the proportion of tertiary butyl alcohol results in a longer retention time of doxycycline and improved separation of doxycycline from the related compounds. Diluent: 0.01 N hydrochloric acid System suitability solution: Prepare a solution of USP Doxycycline Hyclate RS in Diluent containing about 6 mg of doxycycline/mL. Transfer 5 mL of this solution to a 25-mL volumetric flask, heat on a steam bath for 60 min, and evaporate to dryness on a hot plate, taking care not to char the residue. Dissolve the residue in 0.01 N hydrochloric acid, dilute with Diluent to volume, and mix. Pass a portion of this solution through a filter having a porosity of 0.5 µm or finer, and use the filtrate. This solution contains a mixture of 4-epidoxycycline, 6-epidoxycycline, and doxycycline. When stored in a refrigerator, this solution may be used for 14 days. [Note—Throughout the following procedures, protect the Standard solution and the Sample solution from light. ] Standard solution: Transfer 12 mg of USP Doxycycline Hyclate RS, to a 10-mL volumetric flask, add 6 mL of Diluent, sonicate for about 5 min or until dissolved, and dilute with Diluent to volume. Sample solution: 55 mg of Doxycycline in a 50-mL volumetric flask. Add 12 mL of 0.1 N hydrochloric acid, swirl to dissolve, and dilute with Diluent to volume. Filter through a filter of 0.5 µm or finer porosity. Chromatographic system (See Chromatography 621, System Suitability.) Mode: LC Detector: UV 270 nm Column: 4.6-mm × 25-cm; packing L21 Column temperature: 60 ± 1 Flow rate: 1 mL/min Injection size: 20 µL System suitability Sample: System suitability solution and Standard solution [Note—The relative retention times for 4-epidoxycycline (the main degradation product), 6-epidoxycycline, and doxycycline are 0.4, 0.7, and 1.0, respectively. ] Suitability requirements Resolution: NLT 3.0 between the 4-epidoxycycline peak and the doxycycline peak, System suitability solution Tailing factor: NMT 2.0, System suitability solution Relative standard deviation: NMT 2.0%, Standard solution Analysis Samples: Standard solution and Sample solution Calculate the quantity of C22H24N2O8, in µg, in each mg of the Doxycycline taken: Result = (rU/rS) × (CS/CU) × P rU = = peak response from the Sample solution rS = = peak response from the Standard solution CS = = concentration of USP Doxycycline Hyclate RS in the Standard solution (mg/mL) CU = = concentration of the Sample solution (mg/mL) P = = designated potency of doxycycline (C22H24N2O8), of USP Doxycycline Hyclate RS (µg/mg) Acceptance criteria: NLT 880 µg/mg and NMT 980 µg/mg |
2樓2011-03-11 17:18:54
3樓2011-03-11 18:43:28
xiaodu2007693
木蟲 (著名寫手)
藥學(xué)版~龍貓
- PhEPI: 14
- 應(yīng)助: 14 (小學(xué)生)
- 貴賓: 1.009
- 金幣: 2814.8
- 散金: 1819
- 紅花: 12
- 沙發(fā): 4
- 帖子: 2236
- 在線: 253.9小時(shí)
- 蟲號(hào): 504085
- 注冊(cè): 2008-02-15
- 性別: GG
- 專業(yè): 天然有機(jī)化學(xué)
4樓2011-03-11 19:17:08
相關(guān)版塊跳轉(zhuǎn)
我要訂閱樓主 yangxicshe 的主題更新
| 4 | 1/1 | 返回列表 |
| 最具人氣熱帖推薦 [查看全部] | 作者 | 回/看 | 最后發(fā)表 | |
|---|---|---|---|---|
|
[考研] 初試 317 +7 | 半拉月丙 2026-03-20 | 7/350 |
|
|---|---|---|---|---|
|
|
[考研] 一志愿211，0703化學(xué)310分求調(diào)劑 +3 | 努力奮斗112 2026-03-15 | 3/150 |
|
|
[考研] 一志愿重慶大學(xué)085700資源與環(huán)境總分308求調(diào)劑 +7 | 墨墨漠 2026-03-20 | 7/350 |
|
|
|
[考研] 301求調(diào)劑 +10 | yy要上岸呀 2026-03-17 | 10/500 |
|
|
|
[考研] 265求調(diào)劑 +9 | 梁梁校校 2026-03-17 | 9/450 |
|
|
|
[考研] 華東師范大學(xué)-071000生物學(xué)-293分-求調(diào)劑 +3 | 研究生何瑤明 2026-03-18 | 3/150 |
|
|
|
[考研] 一志愿 西北大學(xué) ，070300化學(xué)學(xué)碩，總分287，雙非一本，求調(diào)劑。 +3 | 晨昏線與星海 2026-03-18 | 3/150 |
|
|
|
[考研] 藥學(xué)383 求調(diào)劑 +3 | 藥學(xué)chy 2026-03-15 | 5/250 |
|
|
|
[考研] 一志愿 南京航空航天大學(xué)大學(xué) ，080500材料科學(xué)與工程學(xué)碩 +5 | @taotao 2026-03-20 | 5/250 |
|
|
|
[考研] 086500 325 求調(diào)劑 +3 | 領(lǐng)帶小熊 2026-03-19 | 3/150 |
|
|
|
[考研] 招收調(diào)劑碩士 +4 | lidianxing 2026-03-19 | 12/600 |
|
|
|
[考研] 材料專碩306英一數(shù)二 +10 | z1z2z3879 2026-03-16 | 13/650 |
|
|
|
[考研]
 0854，計(jì)算機(jī)類招收調(diào)劑
+3
|
胡辣湯放糖 2026-03-15 | 6/300 |
|
|
|
[考研] 277調(diào)劑 +5 | 自由煎餅果子 2026-03-16 | 6/300 |
|
|
|
[考研] 301求調(diào)劑 +4 | A_JiXing 2026-03-16 | 4/200 |
|
|
|
[考研] 308求調(diào)劑 +4 | 是Lupa啊 2026-03-16 | 4/200 |
|
|
|
[考研] 一志愿蘇州大學(xué)材料工程（085601）專碩有科研經(jīng)歷三項(xiàng)國(guó)獎(jiǎng)兩個(gè)實(shí)用型專利一項(xiàng)省級(jí)立項(xiàng) +6 | 大火山小火山 2026-03-16 | 8/400 |
|
|
|
[考研] 275求調(diào)劑 +4 | 太陽(yáng)花天天開心 2026-03-16 | 4/200 |
|
|
|
[考研] 東南大學(xué)364求調(diào)劑 +5 | JasonYuiui 2026-03-15 | 5/250 |
|
|
|
[考研] 070303 總分349求調(diào)劑 +3 | LJY9966 2026-03-15 | 5/250 |
|