The purpose of this reported study was to develop and validate an LC-MS/MS method for the quantification of goserelin in a Pheroid® formulation simulated intestinal fluid. Biopharmaceuticals are formulated in drug delivery systems to improve their gastrointestinal stability. Goserelin, a peptide drug was formulated in Pheroid® delivery system and its gastrointestinal stability assessed using simulated intestinal fluid, which required an assay to determine the varying amounts of goserelin remaining after a specific time. Several extraction methods and solvents investigated to extract goserelin from complex matrix led to either poor recovery, peak shape or high background interference. A rapid gradient reversed-phase method coupled to tandem mass spectrometry detection was optimized for the separation and quantification of the extracted peptide. A simple, reproducible and good recovery extraction procedure for goserelin quantification was achieved through simultaneous acetonitrile protein precipitation and water-saturated n-butanol liquid-liquid extraction with water dilution. The method was found to be rapid, specific, precise and accurate, and successfully applied to determine goserelin remaining content in a simulated intestinal fluid, with potential use in other lipid-based formulation evaluated in simulated intestinal fluids.

中文翻译：

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开发和验证用于在模拟肠液中定量Pheroid®制剂中的goserelin的LC-MS / MS方法。

这项报道的研究的目的是开发和验证一种LC-MS / MS方法，用于量化Pheroid®配方模拟肠液中的戈舍瑞林。生物药物配制成药物递送系统，以改善其胃肠道稳定性。肽药物Goserelin是在Pheroid®输送系统中配制的，其胃肠道稳定性使用模拟肠液进行评估，这需要进行测定以确定特定时间后剩余的Goserelin的变化量。研究了几种从复杂基质中提取戈舍瑞林的提取方法和溶剂，导致回收率差，峰形或背景干扰高。结合串联质谱检测的快速梯度反相方法进行了优化，以分离和定量提取的肽。通过同时乙腈蛋白质沉淀和用水稀释的水饱和正丁醇液-液萃取，可以实现简单，可重复和良好回收率的戈舍瑞林定量萃取程序。发现该方法是快速，特异性，精确和准确的，并且成功地用于确定模拟肠液中的戈舍瑞林残留含量，并且在模拟肠液中评估了其他基于脂质的制剂中的潜在用途。