Analysis method of residual monomer acrylamide content in medical polyacrylamide aqueous gel
A technology of polyacrylamide and acrylamide, which is applied in the direction of analyzing materials, measuring devices, and material separation, etc. It can solve the problems of unreasonable sample processing methods, arbitrary operation, ambiguity, etc., and facilitate data exchange and comparison, Effect of high sensitivity and reduced analysis cost
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Embodiment 1
[0016] High-performance liquid chromatographic analysis uses the HPLC instrument of Waters Company, model LC-10ATVP, is equipped with WATERS 2487 ultraviolet detector, uses Shim-pack VP-ODS type C18 reverse-phase chromatographic column of Shimadzu Company, φ4.6×250mm, packing SiO treated with ODS (Octadecylsilyl compound) 2 Microparticles with an average diameter of 4.6μm, an average pore diameter of 12nm, and a specific surface area of 410m 2 / g. Secondary distilled water was used as mobile phase. The column temperature is 25°C. Using an autosampler, inject 20 μL per injection. The injected sample is filtered, and the filter mesh has a pore size of 0.46 μm. The detection wavelength of the UV detector was set at 195 nm. The N2000 chromatographic workstation produced by Zhejiang University was used to control the instrument and read the chromatographic data. Prepare 6 concentrations of standard solutions with recrystallized fresh acrylamide and twice-distilled water, wi...
Embodiment 2
[0017] Get medical polyacrylamide hydrogel sample more than 10g, accurately weigh Wg. Add 20ml of purified acetone, stir, and let stand for 4h. The supernatant was transferred to a rotary evaporator, the water flow pump decompressed, and the temperature was maintained at 36-40°C. After 2 hours of volatilization, the liquid condition is reduced to below 10ml, stop the rotary distillation, transfer the liquid to a volumetric flask with a stopper, and accurately weigh the liquid weight Ww.
[0018] Use the HPLC analysis conditions in Example 1 to carry out unknown sample analysis, read the concentration Cw of acrylamide in the concentrated extract on the calibration curve from the UV detector reading obtained, then use the following formula to calculate the residue in the gel sample Acrylamide content Cg:
[0019] Cg=Ww×Cw / Wg Table 1 is the test results of 3 typical samples. It can be seen that the residual monomer content in them is indeed different.
[0020] typica...
Embodiment 4
[0026] Take by weighing 10g medical hydrogel sample, press the precipitation extraction method among the embodiment 2, after obtaining extract, after the gel that precipitates is swelled to balance (about 6-8 hours) with 10g twice distilled water, add 20ml acetone Precipitation extraction was performed to obtain a second extract. Repeat again to obtain a third extract. The three extracts were evaporated with a rotary evaporator, and the evaporator was decompressed with a water flow pump. The evaporation temperature was controlled at 36-40° C., and the evaporation was carried out until the volume of the residue was less than 10 ml. Accurately weigh the remaining liquid and transfer it to a volumetric flask with a stopper. HPLC analysis was carried out by the method in Example 1. Table 2 compares the results of precipitation extraction 1 time, 2 times and 3 times.
[0027] Table 3 Precipitation Extraction Times Comparison Test Precipitation Extraction Times Resid...
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