Haky J E, Stickney T M
J Chromatogr. 1985 Mar 8;321(1):137-44. doi: 10.1016/s0021-9673(01)90430-3.
A generalized gas chromatographic method is described for the determination of a wide variety of residual solvents and other volatile impurities in bulk pharmaceuticals. The method employs a highly selective graphitized carbon-black stationary phase, which is demonstrated to retain compounds on the basis of a linear combination of their boiling points and molecular volumes (i.e., molecular weight divided by density). An autosampler is utilized to optimize injection precision and to provide for high sample throughput. Analytical data from replicate determinations of seven representative compounds are reported, and it is shown that calibration of the chromatographic systems against external standards produces comparable results to those obtained by standard addition techniques.
本文描述了一种通用气相色谱法，用于测定原料药中多种残留溶剂和其他挥发性杂质。该方法采用高度选择性的石墨化炭黑固定相，经证明，该固定相基于化合物沸点和分子体积（即分子量除以密度）的线性组合来保留化合物。使用自动进样器优化进样精度并实现高样品通量。报告了对七种代表性化合物进行重复测定的分析数据，结果表明，采用外标法对色谱系统进行校准，所得到的结果与标准加入法相当。
