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为了对寡核苷酸固相合成所用的脱保护试剂二氯乙酸做全面的质量控制。实验对二氯乙酸中无机杂质:氯化物、铁盐和重金属等进行了限度控制;建立了离子色谱法含量测定方法。Ionpac AS23(4×250 mm)分析柱;淋洗液为0.8 mmol/L NaHCO3和4.5 mmol/L Na2CO3;抑制型电导检测器。实验结果表明,二氯乙酸的线性方程为:Y=26.01X-0.518 7,(r=0.999 5)。在0.004～1μL/mL浓度范围内呈良好的线性关系,其检测限为0.000 2μL/mL。本方法的精密度和重现性分别为1.26%和0.94%。实验所建立的方法准确,限度合理,能保证二氯乙酸质量和脱保护步骤的顺利进行。
In order to make full-scale quality control of the deprotection reagent dichloroacetic acid used in the oligonucleotide solid-phase synthesis. Experiments on the dichloroacetic acid inorganic impurities: chloride, iron salts and heavy metals were limited control; established a method for the determination of ion chromatography content. Ionpac AS23 (4 x 250 mm) analytical column; eluent was 0.8 mmol / L NaHCO3 and 4.5 mmol / L Na2CO3; inhibitory conductivity detector. The experimental results show that the linear equation of dichloroacetic acid is: Y = 26.01X-0.518 7, (r = 0.999 5). In the concentration range of 0.004 ~ 1μL / mL showed a good linear relationship, the detection limit of 0.000 2μL / mL. The precision and reproducibility of this method were 1.26% and 0.94%, respectively. The method established by the experiment is accurate and the limit is reasonable, which can ensure the quality of the dichloroacetic acid and the smooth progress of the deprotection steps.