毛细管气相色谱法测定伊班膦酸钠中有机溶剂残留量

Determination of Residual Organic Solvents in Sodium Ibandronate by Capillary Gas Chromatography

建立了毛细管气相色谱法测定伊班膦酸钠中的有机溶剂残留量。采用PEG-20M毛细管色谱柱,30 m×0.32 mm,液膜厚度为1.0μm;柱温60℃,维持5 min后,再以30℃/min的速率升温至180℃,维持2 min;FID检测器;正丙醇为内标进行测定。丙酮、甲醇、乙醇、氯苯的线性范围分别为0.04 957～0.9 913 mg/mL(r=0.999 9)、0.030 56～0.611 3 mg/mL(r=0.999 2)、0.050 68～1.014 mg/mL(r=0.999 8)、0.0 038 29～0.076 58 mg/mL(r=0.999 9);平均回收率分别为101.4%、98.58%、98.42%、99.98%;RSD分别为2.40%、1.86%、2.02%、3.78%(n=9);检测限分别为0.25、0.50、0.25、0.11μg/mL。方法快速、灵敏、准确,适用于伊班膦酸钠中有机溶剂残留量的测定。

To establish a capillary gas chromatography method for the determination of residual organic solvents in Sodium Ibandronate. The samples were analyzed with an FID detector using propanol as the internal standard. A 30 m × 0.32 mm PEG - 30M capillary chromatographic column was adopted and the film thickness was 1.0 μm. The ini-tial column temperature was kept at 60℃ for 5 minutes,then raised to 180℃ at the rate of 30℃ per minute,kept for 2 minutes. The standard curves were linear in the range of 0. 04957 - 0.9913 mg/mL（ r = 0.9999 ） for acetone, 0.030 56 - 0.611 3 mg/mL（ r = 0. 999 2） for methanol, 0. 050 68 - 1. 014 mg/mL（ r = 0.999 8） for ethanol and 0.003 829 -0.076 58 rng/mL（ r = 0.999 9）for chlorobenzene. The average recoveries for the four residual organic solvents were 101.4% ,98.58% ,98.42% and 99.98% ,with RSD being 2.40% ,1.86% ,2.02% and 3.78% （ n = 9 ）. The meas- urable lowest limits were 0.2,0.5,0.2 and 0.1 ixg/mL,respectively. The method is rapid, sensive, accurate and can be used to determine the residual orzanic solvents in Sodium Ibandronate.