论文部分内容阅读
目的建立高效液相色谱测定抗人T淋巴细胞猪免疫球蛋白中戊二醛残留量的方法。方法取供试品,与2,4-二硝基苯肼柱前衍生化,过滤,进样。色谱条件:色谱柱采用十八烷基硅烷键合硅胶填充柱;以50%乙腈(乙腈∶水=1∶1)溶液为流动相,流速为0.9 ml/min,检测波长为360 nm,柱温30℃。用该方法检测2批供试品中戊二醛的含量,并确定该方法的检测限、定限量、准确度和精密度。结果该方法检测的2批供试品中戊二醛的含量分别为9.8和7.5μg/ml;该方法的检测限为0.61μg/ml,定量限为2.04μg/ml,在2～20μg/ml范围内,其线性相关系数为0.998 2,检测5、10、15μg/ml戊二醛的回收率分别为102.3%、101.6%和99.2%,相对标准偏差均小于4.0%。结论高效液相色谱法可以简便、准确地检测抗人T淋巴细胞猪免疫球蛋白中戊二醛的残留量,为其生产工艺参数的确定提供了实验依据。
OBJECTIVE To establish a method for the determination of glutaraldehyde residues in porcine immunoglobulin of human T lymphocytes by high performance liquid chromatography. Methods for the test sample, and 2,4-dinitrophenylhydrazine column derivatization, filtration, injection. Chromatographic conditions: column octadecylsilane bonded silica packed column; 50% acetonitrile (acetonitrile: water = 1: 1) solution as the mobile phase at a flow rate of 0.9 ml / min, the detection wavelength was 360 nm, the column temperature 30 ° C. This method was used to test the content of glutaraldehyde in two batches of the test sample and to determine the limit of detection, limit, accuracy and precision of the method. Results The glutaraldehyde content in the two batches of samples tested by this method were 9.8 and 7.5 μg / ml, respectively. The detection limit of this method was 0.61 μg / ml, the limit of quantification was 2.04 μg / ml, The linear correlation coefficient was 0.998 2. The recoveries of 5, 10, 15 μg / ml glutaraldehyde were 102.3%, 101.6% and 99.2%, respectively, and the relative standard deviations were all less than 4.0%. Conclusion High performance liquid chromatography (HPLC) can be used to detect glutaraldehyde residues in porcine immunoglobulin against human T lymphocytes easily and accurately, providing an experimental basis for the determination of production process parameters.