Determination of multiple residual solvents in ibandronate sodium using headspace-gas chromatography

Ibandronate sodium, a third-generation diphosphate drug used worldwide to treat osteoporosis, has the advantages of convenient use, low toxicity, and significant therapeutic effects. However, the residual organic solvents in the synthesis process of sodium ibandronate not only have a negative impact on the efficacy of the drug, but also lead to a decrease in drug stability. Moreover, if the residual amounts of these solvents exceed safety standards, they may pose serious threats to human health. This study successfully established a convenient and efficient method based on headspace-gas chromatography ( HS-GC) for the simultaneous determination of five residual solvents ( methanol, acetone, benzene, toluene, 1-pentanol) in the raw materials of ibandronate sodium. The results indicated that satisfactory analytical performance can be achieved by using DB-624 capillary column ( 30 mx0. 32 mm x 1. 8 mu m) and a flame ionization detector in conjunction with headspace autosampling and a temperature program. The specific operating conditions included an initial temperature of 40 degrees C, with a hold of 2 min, followed by a temperature ramp first to 200 degrees C at a rate of 5 degrees C/min and then to 240 degrees C at a rate of 20 degrees C/min, with a hold of 5 min. Nitrogen with a flow rate of 1 mL/min and split ratio of 14 :1