Transcript Reactorul Nuclear de Cercetare si Productie de

National Institute of C&D
for Physics and Nuclear
Engineering (IFIN-HH)
“Horia Hulubei”
“Gamma Spectrometry and Neutron
Activation Analysis used in Pharmaceutical
products quality control”
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 IFIN-HH
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CPR DEPARTMENT
RESEARCH -PRODUCTION
RADIOISOTOPES AND
RADIOPHARMACEUTICAL PRODUCTS
CENTRE
ANALYSIS LABORATORY
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ANAYSIS LABORATORY
Since 2001
CERTIFICATE LABORATORY
of National Commission for
Nuclear Activities Control (CNCAN)
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Domains of tests
1.Qualitative and Quantitative Physico-chemical Analysis:
•Atomic Absorbtion Spectrofotometry;
•UV-Vis Spectrofotometry;
•Neutron Activation Analysis;
•Gravimetrical and volumetrical methods;
•pH determinations;
2.Radionuclidic analysis –Gamma spectrometry;
3.Radiochemical analysis-radiocromatographyque method;
4.Microbiological analysis (sterility; pirogenity; toxicity;
biodistribution determinations);
5.Activity measurements ;
6.Dosimetrycal measurements
7.Examination of Radioactive sources
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Gamma Spectrometry it’s using in our Laboratory
for:
Radiopharmaceutical Quality Control;
Radionuclidic purity determination;
Activity measurement;
Radionuclides identification;
Radioactive contamination control;
Neutron Activation Analysis
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Gamma Spectrometry
CANBERRA Equipment consist in:
HP Ge detector with preamplificator;
Tension source with (0-4000) V domain;
ACCUSPEC-A multi-channel analyzer ;
PC with analysis program
The detector was calibrated in energy ( 50-1500
keV) domain, using a standards set.
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Radionuclidic purity determination
For principales Radiopharmaceuticals producted in our
Department:
Na131I solution used in thyroidian cancer
radiotheraphy;
Gelatine capsules with Na131I used in thyroidian
affections diagnosis;
99Mo-99mTc ROMTEC Generator for diagnosis
P RN is calculated as proportion between the activity of
specific radionuclide and the sum of all determined
radionuclides activities
PRN for radiopharmaceutical products must be more
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99.9%
Spectrul radiatiilor gama al unei probede solutie Na 131I, MATERIE PRIMA,
puritateradionuclidica depeste 99,99 %(Seria 8/2005, masuraredin 14 mai 2005)
100000
364,49 keV (131I)
80000
Nr.imp.
60000
40000
20000
0
0
500
1000
E (keV)
1500
2000
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Spectrul radiatiilor gama al unei probe de solutie Na 13 1 I, MATERIE PRIMA, avand ca impuritate 13 3 I;
puritatea radionuclidica a 13 1 I este de circa 99,93 % (Seria 12/2004, masurare in 29 mai 2004)
200000
364,49 keV (131I)
Nr. imp.
150000
100000
50000
529,87 keV (133I)
0
0
500
1000
1500
2000
E (keV)
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Spectrul radiatiilor gama corespunzator eluatului de la Generatorul de 99mTc, nr. G4, cu puritate
radionuclidicade peste 99,99% (Lot 14/2003, masurare din 5.10.2003)
600
550
140,51 keV (99mTc)
500
450
Nr. imp.
400
350
300
250
200
739,50 keV (99Mo)
150
100
50
0
0
500
1000
E (keV)
1500
2000
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Neutron Activation Analysis is used in
our Laboratory for:
To determine possible impurities from
not radioactive raw materials;
To determine the content of
microelements in new pharmaceutical
products
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An example of Neutron Activation Analysis
One of our clients had developed a new
pharmaceutical product that had as active
principle -nettle (Herba Urticae);
To determine the content of microelements
in a new pharmaceutical product:
Irradiation condition:
-Flux: 1,1 x 1011n / cm2s
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Target for neutron activation
Closed by welding
h = 100 mm
height = 100 mm
Lead
Aluminium
capsule
Sample
 25 mm
Target for neutron activation
Lead
 25 mm
Sample and standards
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Element
Radioisotopes results
from (n,) reaction
Half time
Gamma ray
(keV)
Scheme factor
Na
24Na
Mg
27Mg
Al
28Al
Cl
38Cl
37.3 min.
1642
32.8
K
42K
12.36 h
1525
17.8
Ca
47Ca
3.4 d
159
70
Sc
46Sc
83.9 d
889
100
V
52V
3.75 min.
1434
100
Mn
56Mn
2.58 h
847
99
Fe
59Fe
1099
56
Co
60Co
1173
100
La
140La
1596
96
15.03 h
1368
100
9.47 min.
1014
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2.31 min.
1778
100
44.6 d
5.27 y
40.3 h
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Element
Unit of
concentration
Leaf
Stem
Root
Uncertainty
(%)
Na
ppm
150
90
6750
5
Mg
ppm
800
940
1370
25
Al
ppm
320
680
2420
25
Cl
ppm
1320
3490
2520
10
K
%
3.34
Ca
%
5.56
Sc
ppm
V
ppm
1
Mn
ppm
45
Fe
%
0.08
Co
ppm
0.5
La
ppm
0.2
-
4.91
1.46
2
-
0,21
2
-
1
30
-
11
50
45
5
20
-
1.5
-
10
2
10
0.6
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Big variations of concentrations from element to element (from ppm to
%) and differences of content for each element on different segments of
plant
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Conclusion:
Gamma Spectrometry and Neutron
Activation Analysis are two very
sensitive methods for pharmaceutical
quality control
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