LC-MS确定双氯芬酸钠含片中的有关物质

LC-MS Identification of Related Substances in Sodium Diclofenac Lozenges

目的:报道了双氯芬酸钠含片中有关物质的 LC-MS 的鉴定方法。方法:采用 LC-MS 测定双氯芬酸钠含片中的有关物质。色谱柱为 C_8(end-capped)柱,流动相为0.5%乙酸溶液-甲醇(34∶66),流速为0.5mL·min^(-1);配有 APCI 离子源的LCQ 型液相色谱离子阱质谱联用仪。结果:参照 BP2002及 USP 28中的双氯芬酸钠的有关物质,根据色谱图、相对分子质量和同位素丰度比确定2个降解产物,并推测出另1个降解产物。结论:本法能够排除辅料的干扰,确定其降解产物,为考察双氯芬酸钠含片的稳定性和控制产品质量确定物质基础。

Objective： A method was described for the identification of related substances in sodium diclofenac lozenges with LC - MS. Methods： HPLC - MS method was employed to determine the relative substances in sodium diclofenac lozenges. The mobile phase was methanol -0. 5% acetic acid （66： 34） , flow rate was 0. 5 mL · min^-1 chromatographic column was C8 （end -capped）. The analytes were detected by electrospray ion trap mass spectrometer with atmosphere pressure chemical ionization source. Results： Consulting the relative substances of sodium diclofenac in BP 2002, two relative substances were identified on the basis of the difference chromatograms of blank and sample, molecular mass and isotopic abundance ratio. Another relative substance was speculated. Conclusion： The method is more specific and accurate. It provides a scientific basis for the detection of stability of sodium diclofenac lozenges and the product quality under control.