Determination of Silicone Oil in Diluent for Suspension of Microspheres for Injection by Nuclear Magnetic Resonance
Objective:To establish a quantitative proton magnetic resonance(qHNMR)method for determination of silicone oil content in the diluent for suspension of microspheres for injection.Methods:The qHNMR were obtained in chloroform-d(without tetramethylsilane)with the internal standard caffeine by a Bruker Avance NEO 600 NMR spectrometer.The parameters of which were set up as follows:the pulse sequence was zg30,the relaxation delay time was 15 s,the number for scanning was 16,and the experiment temperature was controlled at 25℃.The assay of silicone oil was calculated by establishing a standard curve based on the ratio between the quantitative peak areas of silicone oil and the quantitative peak areas of the internal standard with the content of silicone oil.Results:The calibration curve was linear in the concentration range of 6～100 μg with the correlation coefficient(r)of 0.999 9.The average recovery at low,medium and high concentrations was 97.8%(n=9).And the reproducible RSD was 9.8%.Conclusion:The established method for the determination of silicone oil content in the diluent for suspension of microspheres for injection by using qHNMR is relatively convenient and simple,rapid,with high accuracy and sensitivity.
quantitative proton magnetic resonance(qHNMR)diluent for suspension of microspheres for injectionsilicone oilcontentstandard curve method
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