• Korean Journal of Clinical Pharmacy
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• v.16 no.1
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• pp.23-27
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• 2006

Doxorubicin (DXR) is a type of anti-cancer drug called an 'anthracycline glycoside', It works by impairing DNA synthesis, a crucial feature of cell division, and thus is able to target rapidly dividing cells. Doxorubicin is a very serious anti-cancer medication with definite potential to do great harm as well as great good. A liquid chromatography-tandem mass spectroscopy (LC-MS/MS) method was developed to identify and quantify DXR in small-volume biological samples. After the addition of internal standard (IS, $5{\mu}L\;of\;1{\mu}M/ml$ daunorubicin methanol solution) into the serum sample, the drug and IS were extracted by methanol. Following vortex for a 1min and centrifugation at 15,000g for 10 min the organic phase was transferred and evaporated under a vacuum. The residue was reconstituted with $350{\mu}L$ of mobile phase and $10{\mu}L$ was injected into C18 column with mobile phase composed of 0.05M ammonium acetate (0.1 M acetic acid adjusted to pH 3.5) and acetonitrile (40:60, v/v). The flow rate was kept constant at $350{\mu}L/min$. The ions were quantified in the multiple reaction mode (MRM), using positive ions, on a triple quadrupole mass spectrometer. The lower limits of quantification for Doxorubicin in plasma and small tissues were approximately 0.5 ng/mL and 0.5 ng/mL respectively. Intra- and inter-assay accuracy (% of nominal concentration) and precision (% CV) for all analytes were within 15%, respectively.

• Analytical Science and Technology
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• v.29 no.4
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• pp.170-178
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• 2016

Accuracy and precision of ID methods for different spike isotopes of ⁷⁶Se, ⁷⁷Se, and ⁷⁸Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and ⁷⁸Se showed was a bit better than ⁷⁶Se and ⁷⁷Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for ⁷⁸Se, ⁷⁶Se and ⁷⁷Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of ⁷⁸Se isotope spike (over 100 % RSD). ⁷⁶Se and ⁷⁷Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, ⁷⁸Se should be avoided when large amount of Br exists in matrix. Either ⁷⁶Se or ⁷⁷Se would provide accurate results.