5 (1
→ 2) 2 mL 5 mL
0.01 mol/L
(
.
0.21151 mg I
.
1 g
0.4 g [
(C12H17ClN4OSHCl : 337.27)] 100
.
6 12 μm
.
.
.
)
).
1) 50 mg
.
1 g (mg) = (N) (mg) × 6.25 × 1
(g)
1 mL 80 mL
80 85
30
100 mL
8 (KP VIII) [ 1 ]
31
45 50 3 .
2 mL
(40 110 μm
CM- (H
17 cm
.
.
0.5 mL 2
.
1 mL 1-
10 mg
. (
.) 15 mg
0.001 mol/L
100 mL . 1 mL
100 mL . 1 mL
1 mL
3 mL
. 200 μL
.
QT QS .
= (mg) × QT
Q S
100 mL . 1
mL (1 → 5)
100 mL .
30 cm 5 10
μm
.
1.6 g 200 mL
.
.
.
(C6H12O6) 98.0 % .
8 (KP VIII) 2002
32
.
.
.
.
2)
.
pH 4.0 g 20 mL
pH 4.0 6.5.
50 mL
.
:
3.0 mL 2.0
mL 10.0 mL
3.0 mL 50
mL .
50 mL
3 0.01 mol/L
0.60 mL
.
. 0.01 mol/L 1.0 mL
(0.018 % ).
. 0.005 mol/L 1.0
mL (0.024 % ).
0.01 mol/L 0.25 mL
.
6) 5.0 g 2
.
2.0 mL (4 ppm
).
7) 0.5 g 5 mL
2 3
1 mL 1
.
8) 1.5 g 5 mL
5 mL 1 mL
5
5 mL
(1.3 ppm
).
g 100 mL .
0.32 .
, 3 ).
4 g
0.2 mL
80 mL 30
100 mL
20 ± 1
100 mm αD .
(C6H12O6) (mg) = αD × 1087.0
.
95.0 105.0 %
(C6H12O6 : 180.16) .
.
8 (KP VIII) [ 1 ]
33
.
1 g
20 mL .
2 3 5
mL .
2) 1) 10 mL 0.1 g
1 mL 3
.
pH 3.0 6.5
5.0 g
.
2
. 2.0 mL
.
1.5 g
5 mL 5 mL
1 mL
8) .
2.0 mg .
.
10 w/v%
10 w/v% .
(C6H12O6) 4 g
0.2 mL
100 mL 30
20 ± 1 100 mm
αD .
.
.
(KMnO4) 99.0 %
.
.
.
.
.
2.0 g 200 mL
105 2
4 mg .
2) 0.40 g 10 mL
1 mL
5 mL
.
(5 ppm ).
2.0 mL 5 mL
8 (KP VIII) 2002
34
.
).
200
mL . 0.05 mol/L
25 mL 500 mL
(1 →
20) 200 mL 30 35
23 mL
. 55 60 30
.
KMnO4
34.01) 2.5 3.5 w/v% .
0.05 %
.
.
.
.
.
d 20 20 : 1.01
1 mL 1
10 mL
2 mL 1
.
2 0.1 mol/L
2.5 mL
.
2 mL
2 mL
50
mL .
. 2.5 mL
2 mL 50 mL
(5 ppm ).
10
.
mL (3
.
pH 1.0 g 20 mL
pH 7.5 8.5.
10 mL .
2) 0.6 g
. 0.01 mol/L 0.25
mL (0.015 % ).
40 mL .
3.0 mL 50 mL
. 0.005 mol/L
0.50 mL (0.048 % ).
4) 2.5 g 2
.
2.5 mL (10 ppm
).
5) 1.0 g 1
(2 ppm ).
6) 1.0 g 2 mL,
1 mL 1 mL
8 (KP VIII) 2002
40
.
7) 1.0 g 1 mL
3 mL 4
mL 0.2 mL 1
.
8) 0.5 g
. 90 1
. K
.
)
10 mL
100 mL
.
0.1 g
10 mL
100 mL
.
20 μL
(C 6H 5Na 3O 7) (mg)
= (mg) × QT
Q S
30 cm
2 mL 1000 mL
pH 2.5 .
:
5 .
,
.
(C6H5Na3O72H2O : 294.10)
100
.
.
.
pH 7.0 8.5
.
25 mL
10 mL
. 180
2 30 mL
. 0.1
8 (KP VIII) [ 1 ]
41
.
C6H5Na3O72H2O
w/v% .
38
.
.
.
150 mL 60
150 mL
75
mL 100 mL
. 25 mL
700
2 20
mg .
2 0.1 mol/L
1.0 mL
.
6 mL 50 mL
. .
8 (KP VIII) 2002
48
(0.053 % ).
mL 10
30 mL
50 mL . 4 mL
1 mL 50
mL .
. 0.005 mol/L 1.0
mL (0.480 % ).
5) 1.0 g 20 mL
3 mL 2
5 mL 2
2 mL
50 mL .
.
3.0 mL 2 mL
50 mL (30 ppm ).
6) 0.40 g
5)
(5 ppm ).
).
0.6 g
140 160 mL.
1) 0.7 g
0.5 mol/L
10 mL
25 mL
15
.
25 mL
.
25 mL 2
1)
775 825 30
a (g)
.
6 mL 3
5
b (g) .
(SiO 2) (%) = a-b
(g) × 100
50 mL
0.5 mol/L 10 mL
15 .
100 mL
100 mL .
50 mL 50
mL (1 →
2.0 mL pH 10.7
10 mL
0.05 mol/L
.
8 (KP VIII) [ 1 ]
49
.
.
20 mL
.
1) 0.5 g
(1 → 3) 3 mL
20 mL
.
.
()
.
mL
.
15
100 mL
. 10 mL
6 mL 50
mL .
. 0.01 mol/L 0.30
mL (0.021 % ).
mL 10
50 mL .
2.0 mL 1 mL
50 mL .
. 0.005 mol/L
1.0 mL (0.480 % ).
4) 1.5 g 50 mL
5 mL 20
10
mL 2
.
0.45 g
0.45 g, 6 mL
150 mL . 50 mL
.
2.0 mL,
0.15 g, 0.15 g, 2
mL 50 mL (40
ppm ).
.
. 0.02 mol/L
1.0 mL (0.07 % ).
2) 1.0 g
. 0.01 mol/L 1.0 mL
(0.1 % ).
3) 1.0 g 10 mL
2 mL
50 mL 20 mL
10 mL
. 6 mol/L
1 (1 → 20)
1 mL 5
.
4) 1.0 g 50 mL
9 mol/L 10
mL, 10 mL,
20 mL
(5
.
.
5 mL
100 mL 2 mL
50 mL
.
.
8 (KP VIII) [ 1 ]
53
4.5 mol/L 40
mL (3 → 10) 2 mL
.
. 25 mL
(3 ppm ).
100 mL 10 mL
3.0 g
. 5
0.1
mol/L
.
5.585 mg Fe3
.
mL
1 mL
.
30
5 mL 2
2 mL
.
10 mL
. 5
mL 20 mL
100 mL .
5 mL 2 mL 1
1
.
)
1.5 g
300 mL 75
mL 15 mL
. 0.25 g
10 mL 3
187 199 ().
2) (1 → 40)
.
50 mL .
2) 0.50 g
20 mL
0.01 mol/L 0.10 mL
2
. 0.01 mol/L
0.30 mL
.
. 0.01 mol/L 0.80
mL (0.071 % ).
. 0.005 mol/L 1.0
8 (KP VIII) [ 1 ]
55
5) 1.0 g 30 mL
2 mL
50 mL .
.
2.0 mL 2 mL
50 mL (20 ppm
).
6) 0.6 g 5 mL
5 mL
1 mL
5 mL .
(3.3 ppm ).
7) 0.5 g
10 mL 2 mL 2
5
mL 5
20 mL . 5 mL
2 mL 1
.
).
100 mL 8
mol/L 2 mL NN
0.1 g 0.05 mol/L
.
0.05 mol/L
95.0 105.0 %
(Ca : 40.08) .
.
.
.
1) 5 mL
0.7 mL
1 mL 30
1)
.
.
0.17 EU .
3 mol/L 2 mL
150 mL .
0.05 mol/L
20 mL
1 mol/L 15 mL
0.3 g
56
.
21.0 w/v% .
.
.
1 mL 5 mL
3 mL
.
.
d 20 20 : 1.06 1.07
1) 0.05 mL 5
mL 1 mL 8 mol/L
1 mL
.
2) 0.5 mL 10 mL
0.5 mL
.
3) 10 mL 5 mL
5 mL
.
(7 → 10)
105 30
130 134 .
4) 3) 5 mol/L
5 mL
0.65 mL
1 mL 30
.
10 mL
.
195 ()
.
pH 5.5 7.0.
100 mL .
5 mL 20
mL 1 mol/L 5 mL
0.3 mL
2
4 mL 1
. N-(1-)-N'-
10 1 mL
50 mL
.
mol/L 10 mL ,
100 mL . 5
mL
100 mL . 5 mL
20 mL 1 mol/L 5 mL
.
0.10 % (2 g, ).
2 mL
(90 : 10) 1 mL
2.5 mg .
(C 14H 14O 3) (mg) = 10 × C × QT
Q S
(C14H13NaO3) 98.0 102.0 %
.
.
.
(1 → 40000)
.
.
, 10 mL, 100 mm)
1) 1.0 g
20 mL 1 mol/L
5 mL 20 mL, 20
mL 10 mL 3 .
1
.
2.0 mL (20 ppm
).
5.0 mL
.
1 mL 20 mg
.
1 mL, 3 mL 5 mL
100 mL
1 mL
10 mL
8 (KP VIII) 2002
66
.
. ,
(1), (2) (3) 10 μL
cm
. ( 254 nm)
Rf
Rf
(3)
.
(1), (2)
(3) ( 0.1 %,
0.3 % 0.5 % )
2.0 % .
3) 5.0 g
25 mL
15 mL 3
.
0.1 mol/L
2.2
mL (1.0 % ).
3 ).
p-
50 mL
0.1 mol/L
.
C14H13NaO3
%
(C14H13NaO3 : 252.25) .
.
1)
0.25 g
12 mL 1 mL
.
1
pH 7.4 0.1 mol/L 900
mL 2 50
. 45
.
.
8 (KP VIII) [ 1 ]
67
.
2.62 g
1000 mL .
20
.
(C14H13NaO3) 0.275 g
100
mL 10 mL
.
1 mL
2.0 mL
100 mL .
. 1 mL
2.0 mL
100 mL
. 20 μL
(C 14H 13NaO 3) (mg) = 10 × C × QT
Q S
cm 5 μm
,
.
6
1.5 % .
(C33H44N4O10) 98.5 %
.
.
8 (KP VIII) 2002
68
.
.
(3 → 20)
(3 → 20)(1 : 1) 2
8 mL
.
A1, A2, A3
A1/A3 2.47 2.77, A1/A2 3.50
3.90 A2/A3 0.65 0.75.
146 150
10 .
10 mL
. 25 mL
50 mL 1
mL 5
.
: 25 mL 1
mL 10
. 5 mL 4
0.01 mol/L
0.30 mL 50 mL
1 mL (0.021
% ).
2) 2.0 g 2
.
2.0 mL (10 ppm
).
50 mL
. 25 mL 0.01 mol/L
0.50 mL
2
.
10 mL .
1 mL
50 mL . 5
mL
20 mL
.
.
10 μL
.
(9 : 1)
. (
254 nm)
.
, 4 ).
. 40 mg
500 mL . 10 mL
50
mL .
105 2
50 mg
(2 → 75) 150 mL
500
8 (KP VIII) [ 1 ]
69
50 mL
.
AT As .
= (mg) × A T
A S
(C25H36O6) 96.0 104.0 %
.
.
. (
254 nm)
. 10 mL
.
1 mL
.
3) 50 mg
2 mL 5
. (2 →
7) 2 mL 1
.
1181 cm-1, 1085 cm-1 905 cm-1
.
0.1 g, , 10 mL, 100
mm)
2 .
2.0 mL
(20 ppm ).
5 mL
. 2 mL
cm-1 .
181 185
mol/L 10 mL
.
50 mL 5
. 25 mL 0.01 mol/L
0.60 mL
2
.
mL 50 mL .
.
0.01 mol/L 0.40 mL
15 mL 50 mL
(0.024 % ).
4) 1.0 g 2
.
2.0 mL (20 ppm
).
5) 1.0 g 3
(2 ppm).
6) 0.20 g
20 mL .
1 mL
20 mL . 2
mL
20 mL
.
.
10 μL
.
. ( 254 nm)
.
).
1.5 g
0.5 mol/L
40 mL
()
0.25
mol/L ( :
3 ).
.
mg C34H32N4O9
105.0 % (C34H32N4O9 :
640.64) .
.
0.5 g
8 (KP VIII) 2002
80
.
.
2 75
. 60
20 mL 0.8 μ
m .
10 mL 2
mL 1
25 mL .
105 4
0.1 g
1 100 mL .
2 mL 1
100 mL
.
AS .
.
(C 34H 32N 4O 9) (%) = WS × A T
A S
(mg)
20
.
(C34H32N4O9) 1 g
1 mol/L
100 mL
500 mL .
50 mL 2
mL 1 mol/L
50 mL 250
mL .
105 4
80 mg 1 mol/L
50 mL
100 mL . 2 mL
1 mol/L 20
mL 100 mL
.
AT AS .
(C 34H 32N 4O 9) (mg) = (mg) × AT
A S
× 25 2
(C6H5NO2) 99.5 % .
.
.
.
8 (KP VIII) [ 1 ]
81
4 mL
.
2) 20 mg 1000 mL
.
, 235 239 nm
.
A1,
A2/A1 0.35 0.39.
pH 0.20 g 20 mL
pH 3.0 4.0 .
234 238
2) 0.5 g .
0.01 mol/L 0.30 mL
(0.021 % ).
.
0.005 mol/L 0.40 mL
3 mL 50 mL
(0.019 % ).
8 mL 20
mL A
.
5) 1.0 g 2
.
2.0 mL (20 ppm
).
).
0.3 g
50 mL 0.1
mol/L (
: 5 ).
mg C6H5NO2
95.0 110.0 %
(C6H5NO2 : 123.11) .
.
pH : 5.0 7.0
0.1 g
0.3 mL
2 mL .
105 1
234 238 .
.
100 mL
. 10 mL
10 mL
100 mL
. 105
1 0.1 g
8 (KP VIII) 2002
82
100 mL . 10 mL
10 mL
100 mL
.
10 μL
QT, QS .
( C 6H 5NO 2) (mg) = (mg) × QT
Q S
cm 5 μm
(4 : 1)
.
,
6
1.0 % .
.
(C6H6N2O) 98.0 102.0 %
.
.
.
4 mL
.
mL .
243 247 nm
.
A1,
A2/A1 0.63 0.67 .
pH 1.0 g 20 mL
pH 6.0 7.5 .
128 131
8 (KP VIII) [ 1 ]
83
20 mL .
2) 0.5 g
. 0.01 mol/L 0.30
mL (0.021 % ).
. 0.005 mol/L 0.40
mL (0.019 % ).
4) 1.0 g 1
.
3.0 mL (30 ppm
).
.
A .
, 4 ).
50 mg
100 mL . 5 mL
8 mL
100 mL
.
50 mg
100 mL .
5 mL 8 mL
100 mL
.
20 μL
.
(C 6H 6N 2O) (mg) = (mg) × QT
Q S
.
30 cm 5 10 μ
m
.
:
mL 10 mL .
:
: 20 μL
,
.
(C6H6N2O : 122.13)
.
.
pH : 5.0 7.0
6 mL
8 (KP VIII) 2002
84
100
mL .
(
.
2 mL
pH 9.2
10 mL
3 mL 40 60
pH 9.2
2 mL
398 nm
AT AS
.
(C 6H 6N 2O) (mg) = (mg) × AT
A S
(C15H11N3O3) 99.0 %
.
.
,
.
500) 3 mL 0.1 mL
.
2) 20 mg 15 mL
5
.
.
257 261 nm 308 312 nm
.
A1 A2
A1/A2 1.45 1.65.
1) 0.10 g
20 mL
.
2) 1.0 g 2
.
2.0 mL (20 ppm
).
3) 1.0 g 3
(2 ppm ).
4) 0.25 g
(1 : 1) 10 mL
. 1 mL
8 (KP VIII) [ 1 ]
85
2 mL
(1 : 1) 50
mL .
(
(17 :
.
( 254 nm)
.
0.5 % (1 g, 105 , 4
).
0.4 g
40 mL
0.1 mol/L (
).
.
C15H11N3O3
100 mL .
2 mL
2 mL
15 10
mL
(2 → 5) 12 mL
50
mL . 2
mL
.
410 nm
AT AS .
(C 3H 5N 3O 9) (mg)
= (mg) × 0.7487 × A T
A S
× 1 20
.
8 (KP VIII) [ 1 ]
87
Nifedipine
(C17H18N2O6) 98.0 102.0
% .
.
,
.
1) 50 mg 5
mL 5 mL 2
g 5 .
356 nm
.
.
.
.
10 mL 5 mL
6 mL 50
mL .
. 0.01 mol/L 0.30
mL (0.021 % ).
1 mL 50 mL
. .
0.005 mol/L 0.45 mL
(0.054 % ).
4) 2.0 g 2
.
2.0 mL (10 ppm
).
5) 1.0 g 3
(2 ppm ).
6)
. 5.0 g
(5 : 3) 80 mL
0.02 mol/L (
).
mol/L 1.9 mL
.
g
10 mL .
(3 → 500) 500 mL 1
100 .
60 30 mL
0.8 μm
10 mL
.
105 1
25 mg
(4 → 5)
500 mL . 5 mL
500
mL . ,
2 mL
T,
S B . 0.12 mg/mL
10 mL
.
1 mL
25 30
45 .
360 nm, 485 nm
FT, FS FB .
60 65 %
.
.
(C 41H 64O 14) (%) = WS × FT - FB
F S - FB
0.5 mL 30
mL 15 1
mL (C41H64O14) 5 μg
V mL .
10 mL
. 105
1 10 mg
50 mL
100
mL . 5 mL
50 mL 1 mL
100 mL
. ,
(47 → 50) 2 mL
T, S B .
0.12 mg/mL
10 mL
1 mL
30
45 .
8 (KP VIII) 2002
110
(C 41H 64O 14) (mg) = (mg) × FT - F B
F S - FB
20
.
(C41H64O14) 2.5 mg
n- 5
mL
20
20 mL
n-(5 :
5 mL
100
mL .
105 1
25 mg
50 mL
100 mL
. 10 mL
100 mL
. 10
mL
5 mL
10 .
.
590 nm 2
AT As
.
(C 41H 64O 14) (mg) = (mg) × A T
A S
× 1 10
. α 15 mL 0.8 μm
.
.
(C41H64O13) 2 μg
α mL
T30 37 ± 0.5
30 .
60 α 15 mL
α
mL
T60 .
100 2
8 (KP VIII) [ 1 ]
113
. 1 mL
500 mL
37 ± 0.5 60
0.8 μm
10 mL
.
α mL
TS TB .
T30,
T60, TS TB 7 mL
10
.
5 mL
T'30, T'60, T'S
T'B
0.5 mg/mL
4 mL
10 .
0.5 mL
25 30
45 .
395 nm, 560 nm
F30, F60, Fs FB
.
60 85 %
.
.
30 (C 41H 64O 13) (%)
= W S × F 30 FB
F S FB
60 (C 41H 64O 13) (%)
= WS × ( F 60 FB
F S F B
(mg)
0.5 mL
5 mL
5
.
A 30
mL, 20 mL
A
.
B
. A
30 mL 2
B
.
1 mL (C41H64O13) 5
μg
(4 → 5) V mL
20
.
mg
(4 → 5) 100 mL
. 5 mL
(4 → 5)
100 mL
. , (4
→ 5) 2 mL
8 (KP VIII) 2002
114
. 0.2 mg/mL
10 mL
1 mL
25 30 45
.
400
nm, 570 nm
FT, Fs FB .
(C 41H 64O 13) ( mg)
= ( mg) × F T F B
F S F B
20
.
(C41H64O13) 0.5 mg
12.5 mL
10 .
10 mL 20
50
mL .
.
100 2
20 mg
200 mL . 5
mL 10
mL 12.5 mL
50 mL
.
.
= (mg) × Q T
Q S
(C 2H 5OH) (%) = 4 × S W
× HT
HS
W : (g)
(1
m 149 177 μm 4-
.
6
4.0 % .
.
25 mL
10 mL 1 mol/L
5 mL
. A
B 1 mL
.
30
. 5 mL
.
(PO4 1.0 % ).
:
mL (0.10 mg PO4/mL).
A : 5 g
0.5 mol/L
100 mL .
8 (KP VIII) [ 1 ]
117
20 g
100 mL .
3)
20 μL
AT AS (1.0 % )
(C 22H 29FO 5) (μg) = 1000 × C × A T
A S
, 0.4 g, , ).
50 mg
100
mL . 5 mL
50 mL
.
( 40 , 0.67 kPa
)
1 mL 0.5
mg 1
. ( 105
3 )
(1 : 1)
1 mL 50 μg
2 . 1 10.0 mL
2 1.0 mL
100 mL
. 20 μL
.
= 516.41 472.45
× C × AT
A S
cm 5 μm
.
1000 mL
pH 5.4 .
74 : 26 .
: 1.2 mL/
6
1.0 % .
115.0 %
118
.
g 0.86 g
1000 mL (pH 9.0 ).
50 mL
5 mL 50 mL
. 37 45
25 mL
2 .
. 15 mL
.
65 mL
.
45 mL 125 mL
1
100 mL .
15 mL 2
.
( 40 ,
1 mL 30 μg
.
.
20 μL
AS .
(C 22H 30FO 8P) (mg) = 0.1 × C × AT
A S
cm 5 10 μm