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目的采用顶空气相色谱法测定23价肺炎球菌多糖疫苗中乙醇、丙酮及乙醚的残留量。方法采用顶空气相色谱法,以水为溶剂,甲醇为内标,测定23价肺炎球菌多糖疫苗中乙醇、丙酮及乙醚的残留量,并对该方法进行系统适用性、线性关系、检测限与定量限、精密性、准确性验证及初步应用。结果该方法可使待测组分得到良好分离;测定乙醇、丙酮和乙醚的线性范围分别为:2.660～532.000μg/ml(r=1.000 0)、0.530～105.400μg/ml(r=0.999 8)和0.049～9.760μg/ml(r=0.998 9),检测限分别为0.80、0.16和0.01μg/ml,定量限分别为2.66、0.53和0.05μg/ml,精密性RSD值小于5.0%,平均回收率在95.0%～105.6%之间。该法检测3个批号23价肺炎球菌多糖疫苗中乙醇残留量,均未超过《中国药典》三部(2010版)规定的限度。3批疫苗中均未检出丙酮和乙醚。结论顶空气相色谱法操作简便,准确可靠,可用于23价肺炎球菌多糖疫苗中乙醇、丙酮及乙醚残留量的检测。
Objective To determine the residues of ethanol, acetone and ether in 23-valent pneumococcal polysaccharide vaccine by headspace gas chromatography. Methods Residual ethanol, acetone and ether in 23-valent pneumococcal polysaccharide vaccine were determined by headspace gas chromatography with water as solvent and methanol as internal standard. The system applicability, linearity, detection limit and Quantitative limit, precision, accuracy verification and preliminary application. Results The method was able to separate the tested components well. The linear ranges of ethanol, acetone and ether were 2.660 ~ 532.000μg / ml (r = 1.000 0) and 0.530 ~ 105.400μg / ml And 0.049-9.760μg / ml (r = 0.998 9). The detection limits were 0.80,0.16 and 0.01μg / ml, the limits of quantification were 2.66,0.53 and 0.05μg / ml respectively. The RSD value of precision was less than 5.0% Rates ranged from 95.0% to 105.6%. The method of detection of ethanol residues in three batches of 23-valent pneumococcal polysaccharide vaccine did not exceed the limits of the third part of Chinese Pharmacopoeia (2010 edition). Acetone and ether were not detected in the three batches of vaccine. Conclusion Headspace gas chromatography is simple, accurate and reliable and can be used for the determination of ethanol, acetone and diethyl ether residues in 23-valent pneumococcal polysaccharide vaccine.