1、 -HPLC DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD2 1. Reverse Phase CHIRALPAK AD-3R/AD-RH CHIRALPAK AS-3R/AS-RH CHIRALPAK AY-3R/AY-RH CHIRALPAK AZ-3R/AZ-RH CHIRALCEL OD-3R/OD- RH/OD-R CHIRALCEL OJ-3R/OJ-RH CHIRALCEL OZ-3R/OZ-RH CHIRALCEL OX-3R/OX-RH Immobilized
2、 Type CHIRALPAK IA/IA-3 CHIRALPAK IB/IB-3 CHIRALPAK IC/IC-3 CHIRALPAK ID/ID-3 CHIRALPAK IE/IE-3 CHIRALPAK IF/IF-3 Normal Phase CHIRALPAK AD-3/AD-H/AD CHIRALPAK AS-3/AS-H/AS CHIRALPAK AY-3/AY-H CHIRALPAK AZ-3/AZ-H CHIRALCEL OD-3/OD-H/OD CHIRALCEL OJ-3/OJ-H/OJ CHIRALCEL OZ-3/OZ-H CHIRALCEL OX-3/OX-H C
3、HIRALCEL OB-H/OB CHIRALCEL OC-H/OC CHIRALCEL OA CHIRALCEL OG CHIRALCEL OF CHIRALCEL OK Medium Pressure CHIRALFLASH IA CHIRALFLASH IC CHIRALFLASH ID CHIRALFLASH IE CHIRALFLASH IF Protein-based CHIRALPAK AGP CHIRALPAK HSA CHIRALPAK CBH Special CROWNPAK CR(+)/CR(-) CROWNPAK CR-I(+)/CR-I(-) CHIRALPAK QN
4、-AX/QD-AX CHIRALPAK ZWIX(+)/ (-) CHIRALPAK WH/MA(+) CHIRALPAK OP(+)/OT(+) DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD 1. 2. 3. 4. 5. + DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD Daicel (CH 2 Cl 2 ) 1 4/79 DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTDDaicel 5/79 2 DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD IPA,
5、EtOH 0.1-0.3 ml/min 6/79 DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD : DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD9 2. Normal Phase CHIRALPAK AD-3/AD-H/AD CHIRALPAK AS-3/AS-H/AS CHIRALPAK AY-3/AY-H CHIRALPAK AZ-3/AZ-H CHIRALCEL OD-3/OD-H/OD CHIRALCEL OJ-3/OJ-H/OJ C
6、HIRALCEL OZ-3/OZ-H CHIRALCEL OX-3/OX-H AD-H - 3,5- AD-H - 3,5- DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD10 2.1 - Column description: Shipping solvent: n-Hexane/2-propanol solvent mixture (90/10,v/v) 1. column description CHIRALPAK AD-H 2. 3. - 1.4 DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD11 2.1 - 请在连接
7、色谱柱前，按下述要 点彻底 做好溶 剂切换 根据HPLC 系统 中 不 同 的流动 相 ， 采 用不同 的 冲 洗 方法清 洗 所 有 管路， 示意图如下（注意放在溶剂瓶 中的吸 滤头部 分） DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD12 2.1 - A. / - / 1. 60ml - 2. 60ml - 3. 30ml - B. 1. 60ml - 2. 30ml - C. 30ml DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD13 2.2 - 20 20 100% =70:30:0.1 =70:30 =90:10
8、 ADH =70:30:0.1 4.6*250mm 20 60mL 3m 10MPa 5m 5MPa 10m 3MPa / DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD14 2.3 - / / 100% 100% 100% AY-H/AY-3 100% 15% DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD15 3. pH2.0 a.q (HCOOH) /ACN or MeOH Reverse Phase CHIRALPAK AD-3R/AD-RH CHIRALPAK AS-3R/AS-RH CHIRALPAK AY-3R/
9、AY-RH CHIRALPAK AZ-3R/AZ-RH CHIRALCEL OD-3R/OD- RH/OD-R CHIRALCEL OJ-3R/OJ-RH CHIRALCEL OZ-3R/OZ-RH CHIRALCEL OX-3R/OX-RH H2O /ACN or MeOH pH9.0 a.q (20mM NH4HCO3) /ACN or MeOH DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD16 3.1 - a. pH: 2-9 pH 8.0 pH 8 pH9 b. 5-40 pH 7.0 5-25 c. 500mM d. 90% DAICEL CHIR
10、AL TECHNOLOGIES(CHINA)CO.,LTD17 3.2 - 1. 100% 2. / 60:40 (v/v) 3. 100% 0.3ml/min 2 4. Column care/Maintenance DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD18 4. Immobilized Type CHIRALPAK IA/IA-3 CHIRALPAK IB/IB-3 CHIRALPAK IC/IC-3 CHIRALPAK ID/ID-3 CHIRALPAK IE/IE-3 CHIRALPAK IF/IF-3 pH2.0 a.q (HCOOH) /
11、ACN or MeOH H2O /ACN or MeOH pH9.0 a.q (20mM NH4HCO3) /ACN or MeOH DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD19 4.1 - / =90/10 / =60/40 100% 0.2mL/min 5m 5MPa 60mL DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD20 5. Protein-based CHIRALPAK AGP CHIRALPAK HSA CHIRALPAK CBH Special CROWNPAK CR(+)/CR(-) CROWNPA
12、K CR-I(+)/CR-I(-) CHIRALPAK QN-AX/QD-AX CHIRALPAK ZWIX(+)/ (-) CHIRALPAK WH/MA(+) CHIRALPAK OP(+)/OT(+) AGP HSA CBH CR(+)/(-) CR-I(+)/(-) MA(+) WH QN-AX ZWIX(+) DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD21 5.1 AGP 1- pH 4.0-7.0 HSA pH 5.0-7.0 CBH pH 4.0-7.0 pH 15% DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,
13、LTD22 5.1.1 - Step1. 60mL pH Step2. 60mL Step3. Step1. 30mL Step2. 20 AGP,CBH: H2O/IPA=85/15 HSA: H2O/IPA=90/10 Step3. 4 DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD23 5.1.2 - 1. 0.2-0.4mL/min 3 2. / =75/25 0.2-0.4mL/min 3 3. / =85/15 0.2-0.4mL/min 2 AGP 1. 0.2-0.4mL/min 3 2. / =75/25 0.2-0.4mL/min 3 3.
14、 / =90/10 0.2-0.4mL/min 2 HSA 2.5mM 10mM pH3.5 / =85/15(v/v) 1 4mm 0.5ml/min CBH DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD24 5.2 pH1.0-2.0 15% CR(+)/CR(-) pH1.0-2.0 - / / / 70:30:0.5:0.5 30:70:0.5:0.5 1.0% / K + CR-I(+)/CR-I(-) DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD25 5.2.1 - CR(+)/CR(-): CR-I(+)/C
15、R-I(-): / =95/5 Step.1 100mL 80mL Step.2 50mL Step.3 CR(+)/CR(-) 0.5mL/min 1 4 CR-I (+)/CR-I (-) / =95/5 4 CR-I(+)/CR-I(-) DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD26 5.2.2 - Step.1 / =95/5 Step.2 / =50/50 DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD27 5.3 WH 10m -L- 0.250.5mM 0-50 0.25mM MA(+) 3m -L- 0.
16、12mM 0-40 2mM DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD28 5.3.1 - Step1. 80mL Step2. 80mL; Step3. 60mL Step4. MA(+) Step1. 100mL Step2. 60mL Step3. MA(+) DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD29 0.25mM - 10mM +10% 0.3ml/min 3 WH 5.3.2 - 2mM - 15% v/v 0.5mL/min 3 MA(+) DAICEL CHIRAL TECHNOLOGIES(CHI
17、NA)CO.,LTD30 5.4 QN-AX/QD-AX QN-AX: 5 m O-9- ( ) QD-AX: 5 m O-9- ( ) 100% ZWIX(+)/ZWIX(- ZWIX(+) S,S - -2- ZWIX(-) R,R - - 2- 100% DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD31 5.4.1 QN-AX/QD-AX - +1% v/v 20 1504.6mm i.d. 30ml 20 / 50:50 v/v 5-10 PO / 20 / 50:50 v/v / 50:50 v/v DAICEL CHIRAL TECHNOLOGIES(CHINA)CO.,LTD32 5.4.2 QN-AX/QD-AX -
