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目的建立米格列奈钙中6种有机溶剂残留量的分离测定方法。方法采用溶液直接进样气相色谱法,色谱柱为Po-rapak Q填充柱(2 m×3 mm),载气为氮气,以二甲基亚砜为溶剂,测定了米格列奈钙原料药中甲醇、乙醇、二氯甲烷、四氢呋喃、乙酸乙酯与异丙醚的残留量。结果 6种有机溶剂完全分离,在所考察的浓度范围内线性关系良好,其中甲醇的线性范围在0.306 8~30.68 mg.L-1(r=0.999 97),乙醇的线性范围在0.4964~49.64 mg.L-1(r=0.999 9),二氯甲烷的线性范围在0.060 2~6.02 mg.L-1(r=0.999 5),四氢呋喃的线性范围在0.071 5~7.15 mg.L-1(r=0.999 9),乙酸乙酯的线性范围在0.502 3~50.23 mg.L-1(r=0.999 9),异丙醚的线性范围在0.494 5~49.45 mg.L-1(r=0.999 8)。各残留溶剂的精密度实验RSD均小于5%,平均回收率在94.73%~105.47%之间。结论本实验所建立的方法简便、灵敏、准确,可用于米格列奈钙中有机溶剂残留量的测定。
Objective To establish a method for the separation and determination of 6 organic solvents in mitochondrial calcium. Methods Direct injection gas chromatography was used. The column was packed with Po-rapak Q (2 m × 3 mm), the carrier gas was nitrogen and dimethylsulfoxide In methanol, ethanol, dichloromethane, tetrahydrofuran, ethyl acetate and isopropyl ether residues. Results The six organic solvents were completely separated and had a good linear relationship in the range of concentration. The linear range of methanol was 0.306 8 ~ 30.68 mg.L-1 (r = 0.999 97), and the linear range of ethanol was 0.4964 ~ 49.64 mg (R = 0.999 9), the linear range of dichloromethane was 0.060 2 ~ 6.02 mg.L-1 (r = 0.999 5), the linear range of tetrahydrofuran was 0.071 5 ~ 7.15 mg.L-1 = 0.999 9). The linear range of ethyl acetate was 0.502 3 ~ 50.23 mg.L-1 (r = 0.999 9) .The linear range of isopropyl ether was 0.494 5 ~ 49.45 mg.L-1 (r = 0.999 8) . The RSDs of the residual solvents were less than 5% and the average recoveries were between 94.73% and 105.47%. Conclusion The method established in this experiment is simple, sensitive and accurate and can be used to determine the residual amount of organic solvent in mitiglinide calcium.