分析方法验证报告模板

Page 3 of 8
Validation Report No.: MV-0003-R01
Parameter
System Suitability (Date 2)
Instrument
No. Name of Instrument
Code No.
Manufacturer
Type
1
Electric balance
2
HPLC
Code No. JB003.01 JA032-08
Manufacturer Satorius Shimadzu
Type BP301S SPD-10AV VP System
No
.
Name of Reagent
1. d-alpha Tocopherol
2.
Isopropyl alcohol
3.
2) Peak of Vitamin E standard was well resolved from the solvent
2
Specificity
3pe) ak.
No
Na
< 1.19 2 ~ 4 > 6604 2 ~ 4
Conform
5
3 Linearity and Range Correlation coefficient ( r2) ≧ 0.995
Manufacturer
Class
Purity
Lot No.
1. d-alpha Tocopherol
Sigma
W.S 100.00% 57F03031
2.
Isopropyl alcohol
Fischer Scientific
HPLC
***
3.
Acetonitrile
Fischer Scientific
SD = 7360.8545
D=
0.46%
2. Th N=
5.5 ta： 3. Wa Tai
T= W 0.0 af：nd the
Adjustment
6609.00
(Th
e
Pa
Performed
Fai
by
Checked by
XXX Pharmaceutical Ltd.
Analytical Method Validation Report
2.
dl-alpha Tocopheryl acetate standard.
( Chromatogram No.: 42~46)
1) 2)
3) 4)
干
Pa
Adjustment
ss
Performed by
Fai
Checked by
Adjustment
Performed by
Checked by
XXX Pharmaceutical Ltd.
Mobile Phase (Acetonitrile:Isopropyl alcohol<65:35> / Water) = ( 93/7) Column Lichrospher C18 (5um; 4.6x250mm) Flow Rate 1.2mL/min Detector UV @ 285nm Injection Volume
1.0000
6
4
Accuracy
Recovery % = 100 ± 3%
5
R Precision
Int
101.18%
7
0.46%～1.13% 8
0.36%～ 1.16%
8
Remarks Conclusions Performed by
Checked by
Approved by
XXX Pharmaceutical Ltd.
2.
Isopropyl alcohol
Fischer Scientific
HPLC
***
3.
Acetonitrile
Fischer Scientific
HPLC
***
Standard preparation: (205.4mg/50 mL) x (3mL/ 25 mL) = 492.96μg/mL
Chromatographic conditions
Analytical Method Validation Report
Page 2 of 8
Validation Report No.: MV-0003-R01
Parameter
System Suitability (Date 1)
Instrument
No. Name of Instrument
1
Electric balance
Pa Fai
Performed by
Checked by
XXX Pharmaceutical Ltd.
Analytical Method Validation Report
Page 4 of 8
Validation Report No.: MV-0003-R01
Parameter
System Suitability (Date 3)
Pe No:
1
aMke
1757390
an 1754883.33
2
3
4
5
6
1759144 1729487 1742466 R1S752071 1788742
SD = 19889.289
D=
1.13%
2. Th N=
16157
(Th
e
5ta.5
：W
a,h
3.TT=ailing Factor (T) = 0.99
Parameter
Specification
Results Page
Repeatibility：RSD ≦ 2.0 %
< 1.13% 2 ~ 4
1
System Suitability
Ta
Th
1) Chromatogram showed no significant interference from solvent peak.
XXX Pharmaceutical Ltd.
Analytical Method Validation Report
Validation Report No.: MV-0003-R01
Page 1 of 8
Product Title
Vitamin E 800 IU capsule
Par t
Batch No.: XXXXX
(Th
WW
0.0
f： an
Pa Adjustment
Fai
Performed by
Checked by
Parameter
XXX Pharmaceutical Ltd.
Analytical Method Validation Report Validation Report No.: MV-0003-R01
resolved from the solvent peak. ( Chromatogram No.: 11)
3) Chromatogram of Vitamin E 800 IU capsule is similar to the chromatogram
of dl-alpha Tocopheryl acetate Standard (Chromatogram No.: 10)
4) Forced degradation products stressed by Hydrochloric acid, Sodium hydroxide,
fluorescent light, heat, and hydrogen peroxide do not interfere with the peak of
Analytical Method Validation Report
Parameter
Validation Report No.: MV-0003-R01 Linearity and Range
一、RSetasunldta：rd( r2 ≧C0o.n9c9.(5μ)
sol.
g/mL)
(Chromatogram No.: 12~ 16)
JB003.01
Satorius
BP301S
2
HPLC
JA032-08
Shimadzu
SPD-10AV VP System
Reagent
No. Name of Reagent
Manufacturer
Class
Purity
Lot No.
1. d-alpha Tocopherol
Sigma
W.S 100.00% 57F03031
Parameter and Result
Specification RSD ≦ 2.0%
N ≧ 2,000 T ≦ 2.0
Result 0.46% 5798.00 1.13
Calculation (Chromatogram No.: 01~06)
2
3
4
5
6
1601378 1613858 1617322 R1S622399 1616049
Pe No:
1
aMke
1652148
an 1633665.667
2
3
4
5
6
1642473 1625008 1635003 R1S636746 1610616
SD = 14399.201
D=
0.88%
2. Th N=
5ta.5 ：W a,h 3. T= WW 0.0 f：
an
6604
(T
he
(T
Adjustment
20 μ
Parameter and Result
No.
Parameter
Specification
Result
1 Re 2 Th 3 Tai
1. Re
Specification N ≧ 2,000 T ≦ 2.0
Calculation
(ChromatogramNo.: 26~ 31)
0.88% 5609 1.13
Acetonitrile
Reagent
Manufacturer Sigma
Fischer Scientific Fischer Scientific
Class W.S HPLC HPLC
Purity 100.00%
Lot No. 57F03031
*** ***
Standard preparation: (205.4mg/50 mL) x (3mL/ 25 mL) = 492.96μg/mL
No. 1 Re 2 Th 3 Tai
Parameter
Parameter and Result
Specification
Specification N ≧ 2,000 T ≦ 2.0
Result 1.13% 6020 1.08
1.
Calculation
Re
(Chromatogram No.: 47 ~52)
Instrument
No. Name of Instrument
1
Electric balance
2
HPLC
Code No. JB003.01 JA032-12
Manufacturer Satorius Shimadzu
Type BP301S SPD-M10AVP System
No
Reagent
.
Name of Reagent
Validation of dl-alpha Tocopheryl acetate assay Control Procedure:XXX-0000
Ingredient
Each capsule contains 800 IU of dl-alpha Tocopheryl acetate
Date of validation: 07/02/2002
HPLC
***
4.
5.
Standard preparation: (205.4mg/50 mL) x (3mL/ 25 mL) = 492.96μg/mL
6.
(A
Mobile Phase cLeict
Column hro
Flow Rate
1.2mL/min
Chromatographic conditions Detector UV @ 285nm Injection Volume 20 μ
Specificity
Page 5 of 8
1) Chromatogram showed no significant interference from solvent peak.
( Chromatogram No.: 08~09)
2) Peak of dl-alpha Tocopheryl acetate standard eluated at about 18.6 minutes and was well
Peak area
Linear regression
Page 6 of 8
1.
182.08
588039 Lin
2.
364.16
1219766
y = ax + b
3.
546.24
1826970
y=
3373 X -18300.8
Mobile Phase Column Flow Rate
(A cLeict hro
1.2mL/min
No. 1 Re 2 Th 3 Tai
Parameter
1.
No:
Biblioteka Baidu
1
MPeeak Area 1619787 an 1615132.167
Chromatographic conditions
Detector UV @ 285nm Injection Volume 20 μ