ABSTRACT
@#TA method for the content determination of methionine sulfoxide and methionine sulfone in compound amino acid injection (18AA-II) was established in order to investigate their level in 155 batches of this product, and to explore the reason for the generation of these two impurities.The determination was performed on an Agilent Poroshell 120 EC-C18 column with mobile phases of sodium acetate/tetrahydrofuran solution (A) and sodium acetate solution -acetonitrile-methanol (B, 200∶400∶400) (gradient elution) at the flow rate of 0.5 mL/min.The excitation wavelength and the emission wavelength of the fluorescence detector were 233 nm and 441 nm, respectively.The column temperature was 40 °C, and the injection volume was 8 μL.The contents of methionine sulfoxide and methionine sulfone from 155 batches of compound amino acid injection (18AA-II) was determined using this method, and the residual oxygen content was detected by headspace gas analyzer.The results showed that the linear range of methionine sulfoxide and methionine sulfone were 0.128 1-10.250 0 μg/mL (r = 0.999 9) and 0.261 0-10.440 0 μg/mL (r = 0.999 8), respectively.The limits of quantitation were 0.13 μg/mL and 0.26 μg/mL, respectively; the limits of detection were 0.04 μg/mL and 0.09 μg/mL, respectively.RSDs of precision, stability and repetitive test were all lower than 1.3%.The recoveries ranged 98.00%-100.79% (RSD = 1.15%, n = 9) and 98.19%-102.31% (RSD = 1.33%, n = 9).The content level of oxidized related substances from different manufacturers showed significant difference, showing relevance with the residual oxygen content to some extent, yet no significant correlation with the added amount of antioxygen (sodium pyrosulfite).The method is validated to be useful for the content control of methionine sulfoxide and methionine sulfone in compound amino acid injection (18AA-II).It is quite necessary to include the determination of oxidized related substance into the quality specification.Manufacturers should strengthen the control of remaining oxygen in their products.
ABSTRACT
OBJECTIVE： To establish a method for the content determination of 14 elements in Deproteinized calf blood extractives injection. METHODS： Inductively coupled plasma-mass spectrometry （ICP-MS） was adopted. The radiofrequency power was 1 350 W； flow rate of carrier gas （argon） and collision gas （helium） was 1.1 L/min and 4.5 L/min respectively； integration time was 1.5 s； plasma gas flow rate was 18 L/min； depth of sampling was 65 mm； speed of sampling peristaltic pump was 24.0 r/min； data sampling mode was peak-jump acquisition mode； data collection was repeated for 3 times. RESULTS： The linear ranges of Cd， Pb， As， Co， V， Ni， Tl， Ag， Mo， Cu， Cr， Ba and Al were 0.05-50 μg/L （r＝0.999 7）， 0.05-50 μg/L （r＝0.999 7）， 0.05-50 μg/L （r＝0.999 8）、0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 8）， 0.05-50 μg/L （r＝0.999 6）， 0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 5）， 0.05-50 μg/L （r＝0.999 8）， 0.05-50 μg/L （r＝0.999 6）， 0.05-50 μg/L （r＝0.999 6）， 0.05-50 μg/L （r＝0.999 7） and 0.5-70 μg/L （r＝0.999 8）， respectively. The limits of quantitation were 0.003 1， 0.008 9， 0.016 0， 0.025 0， 0.002 1， 0.006 9， 0.038 1， 0.002 1， 0.005 5， 0.002 0， 0.023 1， 0.005 0， 0.002 0， 0.324 9 μg/L， separately. The limits of determination were 0.000 9， 0.002 7， 0.004 8， 0.007 5， 0.000 6， 0.002 1， 0.011 4， 0.000 6， 0.016 5， 0.000 6， 0.006 9， 0.001 5， 0.000 6， 0.097 5 μg/L， separately. RSDs of precision， stability and repeatability tests were all less than 8％. The recoveries were 87.4％-94.3％（RSD＝2.6％， n＝9）， 110.3％-118.2％（RSD＝1.8％，n＝9）， 89.8％-99.7％（RSD＝3.1％，n＝9）， 77.7％-84.4％（RSD＝2.5％，n＝9）， 105.6％-113.4％（RSD＝2.3％，n＝9）， 106.7％-116.5％（RSD＝2.7％，n＝9）， 89.1％-104.5％（RSD＝4.5％，n＝9）， 105.6％-118.6％（RSD＝3.6％，n＝9）， 77.8％-88.0％（RSD＝4.0％，n＝9）， 106.7％-116.1％（RSD＝2.8％，n＝9）， 88.5％-97.1％（RSD＝3.1％，n＝9）， 80.5％-88.6％（RSD＝2.9％，n＝9）， 85.2％-99.4％（RSD＝4.2％，n＝9）， 97.6％-109.3％（RSD＝3.2％，n＝9）， respectively. CONCLUSIONS： The method is simple， accurate. The precision， stability and repeatability of this method are also good. It is suitable for simultaneous determination of 14 elements in Deproteinized calf blood extractives injection.
ABSTRACT
OBJECTIVE:To establish a method for the content determination of carbohydrates in Osseous and cucumis extract injection. METHODS:Ion chromatography was conducted on the column of Dionex CarboPac PA20 with mobile phase of water-1 mol/L Sodium acetate solution-250 mmol/L Sodium hydroxide solution(gradient elution)at flow rate of 0.45 ml/min,column tem-perature was 35 ℃,and injection volume was 10 μl,detector was electrochemical analysis detector. RESULTS:The linear ranges of galactose,glucose,mannose,sucrose and fructose were 0.5-10.0μg/ml(r>0.998 0);RSDs of precision,stability and reproduc-ibility tests were lower than 2%;recovery was 94.8%-99.1%(RSD=0.52%-0.89%,n=9). CONCLUSIONS:The method is sim-ple,fast and accurate,and can be used for the determination of carbohydrates in Osseous and cucumis extract injection.
ABSTRACT
BACKGROUND:Percutaneous kyphoplasty with bone cement injection for repair of multi-segmental thoracolumbar vertebral osteoporotic fractures can restore the compressed vertebral height, correct deformity and reduce complications. OBJECTIVE: To explore the therapeutic effects of percutaneous kyphoplasty with bone cement in patients with multi-segmental thoracolumbar vertebral osteoporotic fractures. METHODS:Eighty patients with multi-segmental thoracolumbar vertebral osteoporotic fractures were enroled, 29 males and 51 females, aged 61-78 year, including 52 case of two-segmental vertebral fractures, 22 cases of three-segmental vertebral fractures, 6 cases of four-segmental vertebral fractures. Al the patients were divided into experimental group and control group randomly. Patients in the control group were given active basic treatment and anti-osteoporosis treatment and stayed in bed. Patients in the experimental group were given percutaneous kyphoplasty with bone cement injection on the above basis. Al the patients were folowed-up 12 months after treatment. Then the Oswesty dysfunction index, Barthel index, visual analog scale score, and theanterior vertebral height and midline height, Cobb angle were compared between the two groups. RESULTS AND CONCLUSION: In the experimental group, the Oswesty dysfunction index, Barthel index, visual analog scale score, and the anterior vertebral height and midline height, Cobb angle were al significantly improved at 3 days, 3 months and 12 months after treatment than before (P < 0.05). In the control group, the Oswesty dysfunction index, Barthel index and visual analog scale score were improved significantly at 3 and 12 months after treatment (P < 0.05), while the anterior vertebral height and midline height were improve dramaticaly at 12 months after treatment (P < 0.05). Compared with the control group, the experimental group showed better the Oswesty dysfunction index and Cobb angle than the control group at 12 months after treatment (P < 0.05), but there were no difference in the other indicators between the two groups. No adverse reactions associated with bone cement material occurred in the experimental group. Taken together, the percutaneous kyphoplasty with bone cement injection can rapidly relieve pain in patients with multi-segmental thoracolumbar vertebral osteoporotic fractures, which can correct kyphosis and improve patient's quality of life.