RESUMO
【Objective】 To investigate the matrix effect on the determination of potency in Recombinant Human Coagulation Factor Ⅷ for Injection (rFⅧ). 【Methods】 Two different detection matrices were used to establish two methods for detecting the potency in Recombinant Human Coagulation Factor Ⅷ for Injection. And the matrix effect on the determination of potency was determined, including specificity, linearity, repeatability, accuracy and intermediate precision. 【Results】 As to the specificity, the recoveries of the two substrates at high vs low concentration level were 112% and 110% vs 104% and 109%, respectively. As to the linearity, in the range of (0.125-1.000) IU/mL, the correlation coefficient between concentration and coagulation time of standard/ sample was higher than 0.99. As to the accuracy/repeatability, the recoveries of two matrices was 104% and 102%, and RSD was 2.4% and 1.9%. As to the intermediate precision, personnel factor of two matrices was 0.72 and 0.23, date factor was 0.79 and 0.85, and RSD(for 12 times) was 4.2% and 3.0%. Comparison of two matrices was as follows: Deviation in test results of 6 batches of rFⅧ was all lower than 5%. There was no significant difference between two matrices. 【Conclusion】 The two matrices for potency detection show good performance including specificity, linearity, repeatability, accuracy, and intermediate precision. They are suitable for the determination of potency in rFⅧ products.
RESUMO
【Objective】 To establish and optimize a method for the determination of aluminum (Al) residue by inductively coupled plasma mass spectrometry (ICP-MS). 【Methods】 Nitric acid solution was used to treat samples and standards. The concentration of nitric acid solution and equipment parameters were optimized, and the specificity, linearity, repeatability, accuracy, detection limit, quantitative limit and intermediate precision of the optimized detection method were investigated to confirm whether it was suitable for the determination of Al residue in human serum albumin. 【Results】 The concentration of nitric acid was 5%, and digest time was 4 h. The equipment condition of ICP-MS was as follows: RF power: 1600 W, sampling depth: 10 mm, atomizer / carrier gas flow rate: 1.0 L/ min, compensation flow rate: 0.5 L/ min, experimental mode: standard mode, integration time: 0.2 s, data acquisition: 3 times. Specificity: The recoveries of Al: 92% (high concentration, RSD=3.5%), 98% (low concentration, RSD=4.9%). Linearity: In the range of (0~40) μg/L, the correlation coefficient between concentration and optical energy signal (CPS) of standard / sample were higher than 0.999 0. Accuracy/ Repeatability: The recoveries of sample (3 concentration): 108% (RSD=4.7%), 110% (RSD=4.9%) and 110% (RSD=2.8%). The detection limit was 0.006 μg/L, and the quantitation limit was 0.019 μg/L. Intermediate precision: personnel factor and date factor, P>0.05, RSD (12 times)=2%. Comparison between ICP-MS and atomic absorption spectrometry (AAS): the deviation between ICP-MS and AAS was 8%, and that of samples was 3%, with no significant difference noticed between the two methods. 【Conclusion】 After optimization, ICP-MS method has shown good performance in terms of specificity, linearity, repeatability, accuracy, detection limit, quantitative limit and intermediate precision, and is suitable for the determination of Al residue in human albumin products of our company.