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NHÓM 11-L01
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123
1.INTRODUCTION
What is 18F-FDG ? How can Acetonitrile appears ?

A radiopharmaceutical used in During 18F-FDG synthesis process, there may

diagnosing cancer, be a small amount of Acetonitrile (ACN)
cardiovascular and neurological solvent left that cannot be completely removed.
diseases.

Limit of influence of ACN ?

According to the pharmacopoeia standards in
British (BP) and US (USP), residual ACN
solvent must not exceed 0.41mg/mL to be safe
for users
 II. INSTRUMENTS AND CHEMICALS
• GC7890B gas chromatograph (Agilent Technologies – USA)
• Flame ionization detector (FID) Detector
• HP-Innowax 19091N-133 capillary column
• Automatic sample injection system
• Automatic evaporation system
• Nitrogen generator NG600A (PEAK) with output pressure of 70psi
• Hydrogen generator PH200 (PEAK) with output pressure of 37psi
• Air compressor
• Online GC control software (Agilent)
• Analytical balance (Bel Engineering) with error ± 0.0003g
• 100mL volumetric flask (Duran schott)
• 50mL beaker (Bomex)
• Micropipet (Rainin) + tip suitable formicropipet
• V-bottom vial 2mL (Agilent)
Your paragraph text
 01 02 03
ACN standard solution: Test sample: Solvent: distilled water for
lot number BCBV0709, 18F-FDG solution injection
purity ≥ 98.0% (Sigma-Alrich) (Fresenius Kabi)

From ACN standard solution, dillute as follow:

Desired
concentration(mg 0.002 0.01 0.02 0.2 0.3 0.4 0.5 0.6
/mL)

Obtained
concentration 0.001920 0.00960 0.01920 0.1921 0.2837 0.3967 0.5094 0.5685
III.CHROMATOGRAPHY CONDITION
Capillary column: length 30m, diameter
0.25mm
Stationary phase: Fused silicon

Mobile phase : Flame ionization detector (FID) 250 C

o

N2, flow rate Injection

1mL/min

o
35 C for 6 mins
o
110 C for 3 mins
1 Specificity
IV. PROCEDURE
2 LOD and LOQ

3 Construct standard curve

4 Test sample analysis

1 Specificity
ACN standard sample 0.3967 mg/mL , test sample and solvent sample were subjected to

chromatography.

Sample Standard sample Test sample Solvent sample

Retention time 3.809 (min) 3.809 (min)

Spectrum of ACN standard
Spectrum of test sample
Spectrum of solvent sample
 The retention time of the standard ACN solution is similar to

the retention time of the 18F-FDG test sample at 3.809

Discussion minutes

The solvent sample has no peaks so it does not affect the

experiment.

The specificity of the analytical method meets the

requirements
2
Limit of detection Limit of quantification
(LOD) (LOQ)
LOD - lowest signal, or the lowest quantity LOQ - lowest concentration of a

to be determinedfrom the signal, that can substance that can be measured with

be observed with a sufficient degree of certainty using standard tests.

confidence

S/N = 3 S/N = 10
 0

S/N=3 at 0,001921mg/mL
LOD: 1.9microgram/mL
: signal height of the analyte:
LOQ: LOD*10/3=6.33microgram/mL
: baseline interference height
 3
Construct the standard curve
Standard ACN 0.3967mg/mL was measured 6 times

Retention time (pA*s)

SD Relative standard deviation RSD of retention time was 0.0198%

RSD(%) =
x < 1% and of the peak area is 4.2691% < 10%.
Because ACN concentration limit is 0.41 mg/mL, we choose the follow comcentration

to construct the standard curve:

Desired concentration Actual concentrations
(mg/mL) (mg/mL)

0.2 0.1921

0.3 0.2837

0.4 0.3967

0.5 0.5094

0.6 0.5685
• Analyze by gas chromatography for each concentration 3 times
• Then we have equation of the standard curve:

y=Ax+b

• x : concentration
• y : peak area ( pA*s )
RESULT

With the result, the correlation coefficient is

r^2 = 0.9983, and the linearity of the method is
confirmed
 4 Test sample analysis
The test sample is analyzed by gas chromatography to get the value of peak area.
Repeat 6 times

SD
RSD(%) =
x
The relative standard deviation RSD of
the peak area reached 1.37% (< 10%)

Acceptable
Substitute into the standard curve equation to get ACN concentration in the test
sample

ACN concentration is around 0.09

mg/mL< 0.19 mg/mL
=> The result is not really accurate
V. CONCLUSION
The analysis method is being
applied in actual quality control
of radioactive pharmaceutical
18F-FDG at the Hanoi
Irradiation Center.
The ACN concentration is around
0.09 mg/mL << 0.41 mg/mL.
Therefore, 18F-FDG produced by
Hanoi Irradiation Center is safe to
use widely.
 Resource Page
XÂY DỰNG VÀ THẨM ĐỊNH PHƯƠNG PHÁP
PHÂN TÍCH TỒN DƯ DUNG MÔI ACETONITRILE
TRONG SẢN PHẨM DƯỢC CHẤT PHÓNG XẠ 18F-
FDG BẰNG SẮC KÝ KHÍ - Tạp chí KHOA HỌC VÀ
CÔNG NGHỆ - Tập 58 - Số 6B (12/2022)

https://doi.org/10.57001/huih5804.102
Thank
you!
Do you have any questions?