| Calcium disodium edetate,also known as disodium calcium EDTA,is a calcium sodium salt of EDTA and a multi-stage ion chelating agent.Calcium disodium edetate does not chelate with calcium in contrast to disodium ediate,another commonly used chelating agent,and thus may prevent hypocalcemia.Calcium disodium edetate exists in the form of main drug in calcium disodium edetate injection.According to the requirements of consistency evaluation of injection,there are many safety risks due to its direct infusion into blood,so the quality control of calcium disodium edetate in injection needs to be cautious.Therefore,it is very important to establish a rapid method for the determination of calcium disodium edetate.The details are as follows:1.Three new methods for the determination of calcium disodium edetate by resonance light scattering spectroscopy based on nonmetallic oxate were established.In front of the room temperature and no complex pre-treatment under the premise of carbonate ion and hydroxyl ions when the mass ratio of 1:3（method A）and sodium metasilicate ion and hydroxyl ions content quality ratio of 1:3,oxalic acid and hydroxyl（method B）between the amount of substance concentration ratio of 1:4（method C）aroused strong resonance light scattering phenomenon.But after adding calcium disodium edetate,their resonant light intensity decreased obviously.With excitation and emission bandwidth of 5.0 nm and scanning speed of 2 000 nm·min-1,method A:The detection wavelength is 265 nm,and the resonance light scattering difference of the system has a good linear relationship with the concentration of calcium disodium edetate(10.0 mg·L-1)in the range of 0.10-4.00 mg·L-1.The linear regression equation is△IRLS=3261.6C+393.02(C is concentration,unit:mg·L-1),correlation coefficient R=0.9991,detection limit 0.0170 mg·L-1.Method B:The detection wavelength was 249 nm,and the resonance light scattering difference of the system showed a good linear relationship with the concentration of calcium disodium edetate(10.0 mg·L-1)in the range of 0.25-2.50 mg·L-1.The linear regression equation is△IRLS=4323.9C-47.039(C is concentration,unit:mg·L-1).Correlation coefficient R=0.9993,detection limit 0.0290 mg·L-1.The method C:The detection wavelength was 273 nm,and the resonance light scattering difference of the system showed a good linear relationship with the concentration of calcium disodium edetate(10.0mg·L-1)in the range of 0.30-1.20 mg·L-1.The linear regression equation was△IRLS=8413.9C+9064.2(C is concentration,unit:mg·L-1).Correlation coefficient R=0.9992,detection limit 0.0058 mg·L-1.2.Two new methods for the determination of calcium disodium edetate by resonance light scattering based on metal oxate were developed.Under the premise of normal temperature and without complex pre-treatment,method D:When the mass ratio of tungstate ion to hydroxide ion was 1:4,strong resonance light scattering phenomenon was caused,but after the addition of calcium disodium edetate,the resonance light intensity was significantly weakened.When the excitation and emission bandwidth was 5.0 nm,the scanning speed was 2 000 nm·min-1,and the detection wavelength was 250 nm,the resonance light scattering difference of the system showed a good linear relationship with the concentration of calcium disodium edetate(10.0 mg·L-1)in the range of 0.50-3.50 mg·L-1.The linear regression equation is△IRLS=3598.5C+1394(C is concentration,unit:mg·L-1),correlation coefficient R=0.9992,detection limit 0.0241 mg·L-1.Method E:Based on REDOX reaction,the resonance light scattering intensity was significantly enhanced after the addition of calcium disodium edetate.When the excitation and emission bandwidth is 5.0 nm and the scanning speed is 2 000 nm·min-1,two detection wavelengths appear,which are267 nm and 395 nm respectively.Whenλex=λem=267 nm,the resonance light scattering difference of the system has a good linear relationship with the concentration of calcium disodium edetate(10.0 mg·L-1)in the range of 0.50-4.50mg·L-1,and the linear regression equation is△IRLS=2494.3C+25191(C is the concentration,unit:mg·L-1),correlation coefficient R=0.9990,detection limit 0.0929mg·L-1;Whenλex=λem=395 nm,the resonance light scattering difference of the system has a good linear relationship with the concentration of calcium disodium edetate(10.0 mg·L-1)in the range of 0.50-4.50 mg·L-1,and the linear regression equation is△IRLS=2288.5C+23885(C is concentration,unit:mg·L-1),correlation coefficient R=0.9992,detection limit 0.0597 mg·L-1.3.A new method for the determination of calcium disodium edetate by resonance light scattering spectroscopy based on organic acid was developed.Under the premise of normal temperature and without complex pre-treatment,method F:Oxalate ions are dissociated from oxalate at p H 5.8.In Clark-Lubs buffer medium,oxalate ions and water molecules undergo molecular self-aggregation and self-assembly reaction to generate oxalate water molecule aggregates to cause resonance light scattering.Calcium disodium edetate dissociate calcium ions at p H 5.8 and coordinate with oxalate water molecular aggregates to form a new supramolecular aggregates,resulting in a significant increase in resonance light scattering intensity.When the excitation and emission bandwidth is 5.0 nm and the scanning speed is 2 000nm·min-1,two detection wavelengths appear,and the detection wavelength is 309 nm.The resonance light scattering difference of the system has a good linear relationship with the concentration of calcium disodium edetate(10.0 mg·L-1)in the range of0.25-1.50 mg·L-1.The linear regression equation is△IRLS=10319C-1908.2(C is concentration,unit:mg·L-1).Correlation coefficient R=0.9991,detection limit 0.0197mg·L-1.4.A new method for the determination of calcium disodium edetate by visible spectrophotometry based on organic reagent complex was established.Under the premise of normal temperature and without complex pre-processing,method G:based on ligand replacement reaction,after adding calcium disodium edetate,two wavelengths appear in scanning.The intensity of visible light is significantly enhanced everywhere at 420 nm,but significantly weakened at 630 nm.Whenλ=420nm,the absorbance difference of the system has A good linear relationship with the concentration of calcium disodium edetate(100.0 mg·L-1)in the range of 2-14 mg·L-1.The linear regression equation is△A=0.0291C+0.0069(C is concentration,unit:mg·L-1).Correlation coefficient R=0.9991,detection limit 0.7392 mg·L-1;Whenλ=630 nm,the absorbance difference of the system has A good linear relationship with the concentration of calcium disodium edetate in the range of 0.5-12 mg·L-1.The linear regression equation is△A=0.1697 C-0.0319(C is concentration,unit:mg·L-1),and the correlation coefficient R=0.9992.The detection limit was 0.1126mg·L-1. |
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