crude cod liver oil - nanomicro techen.nanomicrotech.com/images/my/5.pdf · cod liver oil analysis...
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Detail purification procedure information is available upon request.
Cod Liver Oil
Analysis of crude______________________________________________
Column Agilent GC DB-WAX
Gradient at 10 min 170 ℃
at 16 min 230 ℃
at 26 min 230 ℃
______________________________________________
Purification______________________________________________
Column UniSil® 10-120 C18, 4.6×250 mm
Loading 1.0 ml/ml
Flow rate 1.0 ml/min
Purity / Recovery EPA 98.0% / 70%
DHA 86.9% / 30%
______________________________________________
0 5 10 15 20 25
0
8000000
16000000
24000000
32000000
PA
Min
0 5 10 15 20 250
1200000
2400000
3600000
4800000
PA
Min
0 5 10 15 20 25
0
1000000
2000000
3000000
PA
Min
Crude Cod Liver Oil
1. EPA 57.4%
2. DHA 24.4%1
2
EPA
purity 98.0%
DHA
purity 86.9%
Detail purification procedure information is available upon request.
Aom0977
Analysis of crude___________________________________________
Column UniSil® 5-120, 4.6×250 mm
Mobile phase A = 0.04% H3PO4
B = ACN
Gradient A / B = 91 / 9
Flow rate 1.0 ml/min
Detector UV 203 nm
___________________________________________
Purification___________________________________________
Column UniPS® 10-300, 4.6×250 mm
Loading 1.2 mg/ml
Flow rate 1.0 ml/min
Purity / Recovery 98.0% / 85%
___________________________________________
0 20 40 60 80 100 120-100000
0
100000
200000
300000
400000
500000
600000
700000
mV
Min
Crude
purity 90.7%
0 20 40 60 80 100
0
100000
200000
300000
400000
500000
mV
Min
Purity 99.0%
Detail purification procedure information is available upon request.
NADP
Analysis of crude______________________________________________
Column 4.6×250 mm C18, 5.0 µm
Mobile phase A= 50 mM Tris-CH3COOH pH7.5
B = MeOH
Gradient at 6 min 3% B
at 10 min 10% B
at 12 - 14 min 20% B
Flow rate 1.0 ml/min
Detector UV 260 nm
______________________________________________
Purification______________________________________________
Column UniPS® 40-300, 15×310 mm
Loading 10.0 mg/ml
Flow rate 5.0 ml/min
Purity / Recovery 95.0% / 85%
______________________________________________
0 5 10 15 20
0
20
40
60
80
100
mA
U
Min
Crude
purity 80.0%
0 5 10 15 20
0
400
800
1200
1600
2000
mA
U
Min
Purity 〉95.0%
Detail purification procedure information is available upon request.
Bortezomib
Analysis of crude______________________________________________
Column Agilent 4.6×100 mm C18, 3.5 µm
Mobile phase A = H2O B = MeOH
Gradient at 0 min 10% B
at 25 min 53% B
at 45 min 58% B
Flow rate 1.0 ml/min
Detector UV 270 nm
______________________________________________
Purification______________________________________________
Column UniSil® 10-120, 4.6×250 mm
Loading 3.2 mg/ml
Flow rate 1.0 ml/min
Purity / Recovery 97.0% / 38.9%
______________________________________________
0.0 0.5 1.0 1.5 2.0 2.5
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
AU
Min
Crude
purity 44.5%
0.0 0.5 1.0 1.5 2.0 2.5
0.0
0.5
1.0
1.5
2.0
2.5
3.0
AU
Min
Purity 99%
Detail purification procedure information is available upon request.
Trypsin
Analysis of crude______________________________________________
Column UniSil5-120 C8, 4.6×250 mm
Mobile phase A = 0.1%TFA B = MeOH
Gradient A / B = 64 / 36
Flow rate 1.0 ml/min
Detector UV 280 nm
______________________________________________
Purification______________________________________________
Column Uni®MSP-50S, 15×310 mm
Loading 10.0 mg/ml
Flow rate 8.0 ml/min
Purity / Recovery 87.0 %/ 63%
______________________________________________
0 10 20 30 40
0
30
60
90
120
150
180
mA
U
Min
Crude
purity 52.0%
0 10 20 30 40
0
30
60
90
120
150
180
mA
U
Min
Purity 87%
Detail purification procedure information is available upon request.
Flurbiprofen axetil
Analysis of crude______________________________________________
Column UniSil® 5-120 C8, 4.6×250 mm
Mobile phase A = 0.5% HAc B = ACN
Gradient A / B = 45 / 55
Flow rate 1.0 ml/min
Detector UV 254 nm
______________________________________________
Purification______________________________________________
Column UniSil® 30-120, C18, 4.6×250 mm
Loading 45.0 mg/ml
Flow rate 1.0 ml/min
Purity / Recovery 99.67%/ 82.2%
______________________________________________
0 2 4 6 8 10 12 14
0
100
200
300
400
500
600
mA
U
Min
Crude
purity 85.0%
0 2 4 6 8 10 12 14
0
50
100
150
200
250
mA
U
Min
Purity 99.67%
Detail purification procedure information is available upon request.
Iohexol
Analysis of crude______________________________________________
Column Agilent 5um C18, 4.6×250 mm
Mobile phase A = H2O B = ACN
Gradient 0 min 1%B
60 min 13%B
Flow rate 1.0 ml/min
Detector UV 254 nm
______________________________________________
Purification______________________________________________
Column Uni®PSN 60-300, 15×310 mm
Loading 75.0 mg/ml
Flow rate 5.0 ml/min
Purity / Recovery 99.6%/ 79%
______________________________________________
0 20 40 60
0
500
1000
1500
2000
2500
mA
U
Min
Crude putiry
98.5%
0 20 40 60
0
100
200
300
400
mA
U
Min
Purity 99.67%
Detail purification procedure information is available upon request.
Iopamidol
Analysis of crude______________________________________________
Column 5um SBC C18, 4.6×250 mm
Mobile phase A = H2O B = 25% MeOH / H2O
Gradient 0 - 6 min 8%B
18 min 35%B
30 - 34 min 92%B
Flow rate 1.5 ml/min
Detector UV 240 nm
______________________________________________
Purification______________________________________________
Column Uni®PSN 30-300, 15×310 mm
Loading 100.0 mg/ml
Flow rate 5.0 ml/min
Purity / Recovery 99.96%/ 94%
______________________________________________
0 10 20 30 40
0
1
2
AU
Min
Crude purity
95.14%
0 10 20 30 40
0
1
2
AU
Min
Purity 99.96%
Detail purification procedure information is available upon request.
Acarbose
Analysis of crude
______________________________________________
Column UniSil® 5-120 C8, 4.6×250 mm
Mobile phase A = ACN B = PBS Buffer
Gradient A / B = 75 / 25
Flow rate 1.0 ml/min
Detector UV 210 nm
______________________________________________
Purification
______________________________________________
Column UniRPC 40-SCX, 15×310 mm
Loading 30.0 mg/ml
Flow rate 8.0 ml/min
Purity / Recovery 98.0%/ 69%
______________________________________________
粗品67%
纯化后 98.5%