Objective: To establish a method for determining molecular weight and distribution of raw mannatide and its preparation with SEC-RI-MALLS. Methods: Specificity,accuracy, precision and robustness of SEC-RI-MALLS method was verified by performing on a Shodex OHpak SB-804 HQ column with 0.05 mol·L-1 sodium sulfate buffer as mobile phase at a flow rate of 0.5 mL·min-1 and a comparison between SEC-RI-MALLS and GPC was studied too. Resulst: The tablet excipient starch had no interference to the test. The relative accuracy error between the measured value and the labeled value of dextran standard was less than 3.0%. RSD of precision was 0.40% when the sample concentration was 2 mg·mL-1 and the RSD of reproducibility and robustness were less than 5.0%. There was no significant difference between Shodex OHpak SB-804 HQ column and TSK-GEL G4000 PWXL column by comparing the results of 79 batches of samples. Compared with the national standard method (GPC) for molecular weight determination, the molecular weight of SEC-RI-MALLS method was 19 509 Da higher on average, and the molecular weight distribution was more concentrated. Conclusion: SEC-RI-MALLS method can determine the molecular weight and distribution of mannatide without standard with good accuracy and robustness. Compared with the existing method, SEC-RI-MALLS method is more conducive to the safety and effectiveness control of the variety.
ZOU Jian, YANG Lei, LIN Tao, WANG Jue-xiao, MA Jin, CHEN Jie, LI Yan
. Determination of molecular weight and distribution of mannatide by means of SEC-RI-MALLS[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(2)
: 256
-263
.
DOI: 10.16155/j.0254-1793.2024.02.08
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