蛋黄卵磷脂在中国药典标准中残留溶剂测定方法的优化

Optimization of Residual Solvent Determination of Egg Yolk Lecithin in Chinese Pharmacopoeia

关键词:  蛋黄卵磷脂  残留溶剂  顶空气相色谱法

Key words:  egg yolk lecithin  residual solvent  headspace gas chromatography

摘要:

目的 建立顶空气相色谱法测定蛋黄卵磷脂中的石油醚、乙醇、乙醚、丙酮、正己烷共5种残留溶剂的含量，并采用气相色谱-质谱联用技术，结合质谱数据检索对样品中的其他挥发性杂质进行结构鉴定。方法 GC条件为色谱柱：DB-624UI毛细管柱(60 m×0.25 mm，1.4 μm)，采用程序升温；检测器：氢火焰离子化检测器；检测器温度：250 ℃；分流比：20∶1。GC-MS条件为GC条件的载气：氦气、不分流模式进样，其余条件同上述GC条件。质谱条件的离子源温度：230 ℃；接口温度：230 ℃；采用电子轰击离子源；电离能量：70 eV；扫描方式：Q3Scan；扫描范围：m/z 45~500；检测时间：7~28.5 min。结果 5种溶剂的分离度良好，样品中其他挥发性杂质对5种待测组分的检测无影响；5种成分在各自浓度范围内呈良好的线性关系(r>0.999)；检测限范围为(0.003~0.13)μg·mL^–1，定量限范围为(0.017~0.21)μg·mL^–1；平均回收率为93.74%~104.31%；精密度、重复性的RSD均<5%。结论 本方法操作简便、灵敏度高，可以用于测定蛋黄卵磷脂中的残留溶剂。

Abstract:

OBJECTIVE To establish a headspace gas chromatography method for the determination of five kinds of residual solvents in egg yolk lecithin, such as petroleum ether, ethanol, diethyl ether, acetone and n-hexane. Using gas chromatography-mass spectrometry technology, the mass spectrometry retrieval data for other volatile impurities in the sample were combined to identify the structure. METHODS GC conditions were column: DB-624UI capillary column(60 m× 0.25 mmm 1.4 μm), the column temperature was raised by program; Detector: flame ionization detector; detector temperature: 250 ℃; Split ratio: 20∶1. GC-MS conditions were GC conditions: the carrier gas was helium, the remaining conditions accorded with GC conditions above. MS conditions were ion source temperature: 230 ℃; the interface temperature was set at 230 ℃; using electron impact inoization; EI energy: 70 eV; scanning mode: Q3Scan mode; scan range: m/z 45-500; detection time: 7.00-28.50 min. RESULTS The 5 residual solvents tested were completely separated, other volatile impurities in the sample had no influence on the 5 residual solvents. The linear relationship was good in the concentration range(r>0.999); limit of detection were (0.003-0.13)μg·mL^-1, limit of quantitation were (0.017-0.21)μg·mL^-1; average recoveries were 93.74%-104.31%; accuracy and repeatability were <5%. CONCLUSION The method is simple, highly sensitive and reproducible, it can be used to determine the residual solvents in egg yolk lecithin.