使用安捷伦7697a 顶空进样器进行美国药典残留溶剂的分析
TRANSCRIPT
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7697A USP
Roger L. Firor
2850 Centerville Rd
Wilmington, DE 19808-1610
USA
7697A 7890 GC UPS 1
2 1 2A 2B RSD% 2.5%
/ 10 mL
20 mL
FID-FID FID-MSD
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2
1 2A 2B
250mL 500mL Brand 6mL 10mL 20mL
Teflon
1 5190-0490
2A 5190-0492
2B 5190-0513
7697A 0.45mm (Restek Siltek
10018) /
2mm SilTite VI
30
0.32mm
7697A (PCM)
EPC 7890
1ml
PCM (NTP)
1 1
(QA) (USP) [1]
/
ICH Q3C
(API)
GC USP
USP USP
GC
USP 1 2
1. A
2. B
3. C
A G43 624 VF-
624ms DB-624 123-1334 B
G16 HP-INNOWax 9091N-113
624 RSD FID (624
NNOWax ) FID/MSD
USP 467
7697A
USP A 7697A 7890
GC //
2mm 5181-
88180 4mm 2103003
FID
VI
/ EPC624
7697A
1.
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7697A 13
1.
2. 3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
EPC
EPC
7697A
2 3
/ 140 C 5:1
145 C 5:1
EPC EPC
0.45 mm
p/n CP9104 30 m 0.32 mm 1.80 m VF-624 ms
40 C (5 min) 240 C (2 min)18 C/min
85 C
/ 85 C
100 C
10 mL 20 mL
1 mL 1 mL
40 min 40 min
0.5 min 0.5 min
15 psia (NTP) 15 psia (NTP)
0 10 psia (NTP)
0.10 min 0.10 min
0.05 min 0.05 min
50 mL/min 50 mL/min
20 psi/min 20 psi/min
2 2
1.
PS1
GC
PCM
6
MFS
/
PV1
PV2
PV
OFF
SV1
ON
3
1
2
4
5
6
2. PCM EPC 6 (SV1) GC EPC 6GC
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4
3. PS1PV2 PCM EPC2
PCM
MFS
PV1
PV2
PV
SV1
ON
OFF
PS1
/
3
1
2
4
5
6
6
GC
ChemStation 7697A
4
4. 20 mL15psi (NTP) 20 psi/min 10 psi (NTP)
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5
2 1 2A 2B USP
RSD 20
10ml20ml /
10ml20ml
RSD 2.5%
(RSD) RSD
k USP
DMSODMACDMI
DMSO
RSD RSD
7697A
2.0 psi (NTP) 10.0 psi (NTP)
7697A
K 7697A
200 mL/min
5
VF-624 ms 1 1,2-
VI
10 mL 20 mL 10 mL 20 mL
1
1,1- 2.9 2.0 2.0 2.6
1,1,1- 2.7 2.2 1.9 3.9
3.8 4.4 3.1 3.4
3.9 2.3 1.5 3.1
1,2- 1.6 1.3 1.1 1.7
2A
1.0 0.6 1.3 0.4
1.0 0.5 1.3 0.6
1.2 1.9 1.5 2.3
-1,2 2.4 2.5 2.9 2.8
-1,2 1.5 2.1 1.8 2.8
0.8 0.6 1.4 0.7
3.5 2.9 4.2 2.9
4.1 3.9 4.3 3.2
1,4- 1.4 0.6 1.6 0.5
1.5 2.0 2.1 2.8
1.4 2.1 1.7 3.0
1.6 2.2 2.1 2.7
/ 1.6 2.2 2.0 2.9
1.4 2.2 1.8 3.1
2B
3.9 1.3 3.6 2.7 5.4 4.8 4.4 3.3
4.0 2.5 1.7 1.7
1,2- 1.7 1.6 4.2 4.5
5.9 2.5 2.1 1.6
1.7 0.8 1.5 0.9
2- 1.5 0.7 0.9 0.7
2.7 2.7 1.4 1.7
2. RSD
n = 20
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5. USP 46712A2BABC/20 mL
1. 1. 1,1,-2. 1,1,1-3. 4. 5. 1,2-
A
12
3
4
5
1. 2. 3. 4. -1,25. -1,26. 7. 8. 9. 1,4-10. 11. 12. 13. /14.
B
1 2
3
4
5
6
7
8
9
10
11
12
13
14
1.
2.
3.
4. 1,2-
5.
6.
7. 2-
8.
1
2
3
4
5
6
7 8C
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6 VF-624ms
INNOWax
1:1 30 m 0.32 mm 624 INNOWax UPS
A B SilTite
CFT
6
1 2A 2B 7 8 9
7:1 14psi40
40 5min 18/min 240
2min 10
INNOWax
FID
VI
/EPC
FID
624
7697A
6.
7. USP 4671
1. 1,1,-
2. 1,1,1-
3.
4.
5. 1,2-
1 2, 3 4
5
1
2
3
4
5
INNOWax
624
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8. USP 4672A
9. USP 4672B
1. 2.
3.
4. 1,2-
5.
6.
7. 2-
8.
INNOWax
624
1
2
3
4
5
6
7
8
1
2
3
4
5
6
7 8
1. 2. 3.
4.
-1,2
5. -1,26. 7. 8. 9. 1,4-10. 11. 12. 13. 14. 15.
1
2
3,64 5
7
8INNOWax
624
15
14
1112
13
9
10
1
2
3 4 5 6 7 8
9
10 11 15
12
13, 14
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USP 1 2 624
INNOWax
FID MS 5975C MSD
11 USP
MSD 60
3
10. 5:135 17min 20/min 2405min
624
1. 2. 1,1,-34. 5. -1,26. 7. -1,2, 8. 9. 10., , 1,1,1-
11. 12. 1,2-13. 1,2-14. 15. 16. 1,4-17. 18. 19. 2-20. 21. 22./23. 24.
INNOWax
1. 2.1,1 3. -1,2, THF, 1,1,1- 4. , 1,2 5. , 6. -1,2
, 7. 8. 9. 10. 1,4-11. 1,2-12. 2-13. 14.15.16. ()
17. 18. 19. 20.
Aux EPC not ready
Aux
3
[2]
MSD** FID
40 C 3.5 3.8 4.3 8.1 4.6
150 C 3.5 2.5 2.6 5.1 1.6
240 C 3.5 1.9 1.9 3.8 0.3 *
3. 10 (mL/min)
* Aux EPCnot ready
** 22017.1 cm MSD
INNOWax
624
2019
18
1713, 14, 15
16
12
11
10
9
8
76
5
4
1
2
3
1
2
4
3 5
6 7
810
11
12
13
14 15
1617
18 20, 21, 22, 2319
24
9
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FID MSD 1,4- 2-
MSD
SIM
Aux EPC FID
MSD
4.0 psig
14.7 psi
0 psi
+ Aux = F1 + F2
30 M 0.32 mm 1.80 6 24
Aux EPC
S/S
F1
F2
11. FID-MSD
FID= 80 cm x 0.20 mm
MSD= 137 cm x 0.18 mm
DB-62430 m x 0.32 mm x 1.80 m
12. 2AFID-MSD 20 mL
TIC
FID
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7697A
0.1
EPC
QA USP ICH
FID-MSD
SIM
1. USP 32-NF 27, General Chapter USP Organic
volatile impurities, United States Pharmacopeia.
Pharmacopoeia Convention Inc., Rockville, MD, 8/2009
2. www.agilent.com/chem/flowcalculatorGC
Pressure Flow Calculator Software Revision 2.05
3. Albert E Gudat and Roger L. Firor, Improved Retention
Time, Area Repeatability, and Sensitivity for Analysis ofResidual Solvents, 5989-6079CHCN
www.agilent.com/chem/cn
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www.agilent.com/chem
2011
2011 3 15
5990-7625CHCN