Applications Of Inductively Coupled Plasma-Atomic Emission Spectrometry And Atomic Absorption Spectrometry In Drug Quality Control

Inductively coupled plasma-atomic emission spectrometry is an important technique in element analysis, and has been widely applied in many analysis area including chemical industry, geological minerals, metal materials, electronic products, environmental protection and biological samples, etc, thanks to its many advantages such as low detection limit, high precision, wide dynamic linear range and simultaneous determination capability of many elements. At present, the application of ICP-AES is still less in the quality control for domestic drug, especially chemical drug, but its outstanding technical advantages determine the broad application prospect in this area.In this thesis, the practical applications of ICP-AES in drug quality control were studied, which mainly included two parts of contents:one was the content determination of added elements, the other was the limit test of impurity elements. In addition, atomic absorption spectrometry was applied to the determination of some highly toxic elements, which was regarded as the supplement to ICP-AES. The main contents are summarized as follows:1. A new inductively coupled plasma-atomic emission spectrometry method was established for the simultaneous content determination of four elements consisting of potassium, sodium, calcium, magnesium in Kabiven PI. The samples were directly determined by one single dilution, and the emission lines of K, Na, Ca, Mg were766.490nm,589.592nm,422.673nm,285.213nm, respectively. In a certain concentration range, the emission intensity of K, Na, Ca, Mg and the concentration all showed good linear relationship, with the recoveries of98.3%.98.8%,99.1%,98.4%. The limits of quantification were0.003,0.003,0.001,0.001μg/ml, respectively. The method is specific, sensitive, accurate and simple, and can be used for the content determination of potassium, sodium, calcium, magnesium in similar injection.2. An inductively coupled plasma-atomic emission spectrometry method was established to determine the residue of palladium which was used as a catalyst in one chemical bulk drug, nebivolol hydrochloride. Microwave digestion was used for sample pretreatment, and the detection wavelength was340.458nm. The ICP-AES determination results were compared with those by graphic furnace atomic absorption spectrometry. The emission intensity and the concentration showed a good linear relationship in the10-100ng/ml concentration range, with the relative standard deviation of repeatability1.6%, the recovery94.2%. and the limit of detection0.5μg/g. The method is specific, sensitive, accurate and rapid, and can be used for the determination of catalyst Pd residue in chemical bulk drugs.3. An inductively coupled plasma-atomic emission spectrometry method was established to determine nineteen elemental impurities in chemical bulk drugs simultaneously by choosing gliclazide and iohexol as research object. Microwave digestion and direct dissolution were respectively used to prepare sample solutions according to the solubility properties of gliclazide and iohexol. All elements were divided into three systems in order to overcome the spectral interference between them and guarantee the sensitivity of determination. The appropriate emission lines and the observation mode of every element were determined, and the plasma parameters were optimized. The emission intensity and the concentration of every elements showed a good linear relationship in certain concentration range, and the correlation coefficients were all greater than0.999. The recoveries were76.6%-123.0%from gliclazide. and90.5%-110.7%for iohexoL and the detection limits all met the requirements of determination The method is specific, sensitive, accurate and rapid, and can be used as a universal method for the determination of elemental impurities in chemical bulk drugs to replace the traditional method for heavy metals.4. A new method was established to determine total mercury in chemical bulk drugs by choosing lamivudine and sulfamethoxazole as research object. Hg was determined by cold vapor atomic absorption spectrometry, using microwave digestion for sample pretreatment. The detection wavelength was253.7nm. The absorbance and the concentration showed a good linear relationship in the3.75-18ng/ml concentration range, and the correlation coefficient was0.9996. The recovery of Hg in lamivudine and sulfamethoxazole were96.9%and112.7%, respectively, and the limit of detection was0.02μg/g. The method is specific, sensitive, accurate and rapid, and turns out a universal method for the determination of total mercury in chemical bulk drugs, simultaneously serving as a basis for drug quality control.