The expression radionuclide in nuclear medicine is preferred than radioisotope which widely used in physics. Radionuclides have been used regularly in nuclear medicine. Their radiation provide information about the staging of a person’s specific organs and to specify what is triggering the symptoms, injury or disease to treat diseased organs or cancerous tumours in a patient called theranostic. Technetium-99m radionuclide is the most frequently used radionuclide in nuclear medicine. The quality control of technetium-99m (99m Tc) product from 99Mo/99mTc generator is crucial. One that have been highlighted in this paper is the radionuclide molybdenum-99 (99Mo) breaktrough which can be effectively measured using caliberated gamma spectrometer. The stability test of the gamma spectrometer detector is done using control chart and chi square method from 137Cs radionuclide measurement. The calibration process of liquid standard sources of mix 133Ba, 137Cs and 60Co including energy and efficiency calibration, are performed with the same geometry as Mo99 breakthrough measurement in a lead shield canister with 2.5; 4.5 and 8.5 cm distance from the HPGe detector. The result from the calibration of liquid standard sources of mix 133Ba, 137Cs and 60Co showed the required polynomial equations needed to calculate the 99Mo breakthrough of 99mTc eluted product from the 99Mo/99mTc generator.