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目的:通过对比实验研究是否可以通过优化操作步骤提高滴定法测定一般生物制品中硫柳汞含量的准确性、重复性、降低检测限,并确定控制点。方法:以中国药典2010年版三部附录VⅡB所载滴定方法为基础,细化或调整若干步骤具体操作。结果:优化控制点:①延长水浴消化时间至4 h;②滴定过程中双硫腙滴定液始终保持在约0℃、几乎完全避光、防空气的条件下,逐次取用,使用时长不得超过120 min;③加入滴定液后应充分振摇并适当延长时间;④实验中可根据样品中硫柳汞含量适当稀释双硫腙滴定液,最低至药典所载配比的2/10。结论:经优化,滴定法可达到回收率在90%～110%、RSD≤5%、检测限最低至0.6μg.mL-1。
OBJECTIVE: To compare the accuracy and repeatability of titrimetric method for the determination of thimerosal in general biological products by optimizing the operation procedure through comparative experiments and to reduce the detection limit and to determine the control points. Methods: Based on the titration method described in the three Chinese Pharmacopoeia 2010 edition, Appendix VIIB, the detailed operation of several steps was refined or adjusted. Results: The optimized control points: ① prolong the digestion time of the water bath to 4 h; ② the dithizone titration solution kept at about 0 ℃ during the titration process, almost completely avoid the light, take the anti-air conditions, 120 min; ③ after adding the titration solution should be fully shaken and extended the appropriate time; ④ In the experiment, the dithizone titration solution can be appropriately diluted according to the thimerosal content in the sample to the lowest of 2/10 in the formula. Conclusion: The optimized titration method can achieve a recovery of 90% -110% with RSD≤5% and a detection limit of 0.6μg.mL-1.