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目的:建立气相色谱-质谱联用技术同时测定口服液体制剂中16种邻苯二甲酸酯类塑化剂的检测方法。比较液-液萃取和固相萃取对液体制剂的净化效果影响,并对操作参数进行优化,建立最佳试验条件。方法:分别采用液-液萃取和固相萃取两种样品前处理方式处理样品,采用选择离子监测,以碎片的丰度比定性,外标法定量。结果:采用液-液萃取方法前处理样品时基质的干扰大,杂质峰较多,故采用固相萃取方式对样品进行前处理,GC-MS检测口服液体制剂中16中邻苯二甲酸酯类塑化剂残留量,该方法检出限为0.02μg·g-1,在0.5~8.0μg·ml-1范围内,线性良好(相关系数r范围0.990 7~0.999 8),加标回收率在71.7%~95.6%范围内,RSD为2.1%~9.7%。结论:采用固相萃取,GC-MS的方法对口服液体制剂中16中邻苯二甲酸酯类塑化剂进行检测,方法简便、快速、准确、灵敏度高,适用于口服液体制剂中16中邻苯二甲酸酯类塑化剂的测定。
Objective: To establish a method for the simultaneous determination of 16 phthalate plasticizers in oral liquid by gas chromatography-mass spectrometry. The effects of liquid-liquid extraction and solid-phase extraction on the purification of liquid preparation were compared, and the operating parameters were optimized to establish the optimal experimental conditions. Methods: Samples were treated by liquid-liquid extraction and solid-phase extraction, respectively. The samples were selected by ion monitoring. The abundance ratio of fragments was qualitatively determined by external standard method. Results: The sample was pretreated by liquid-liquid extraction with large interference and impurity peaks. The samples were pretreated by solid-phase extraction. The contents of 16 phthalates The detection limit of this method was 0.02 μg · g-1. The linearity was good in the range of 0.5-8.0 μg · ml-1 (correlation coefficient r ranged from 0.990 7 to 0.999 8). The recoveries were in the range of From 71.7% to 95.6%, RSD ranged from 2.1% to 9.7%. Conclusion: The method of solid-phase extraction and GC-MS for the determination of 16 phthalate plasticizers in oral liquid preparations is simple, rapid, accurate and sensitive. It is suitable for the determination of 16 ortho-phthalates in oral liquid preparations Determination of phthalate plasticizers.