HPLC-MS测定多不饱和脂肪酸微胶囊粉剂中的壬基酚

建立了多不饱和脂肪酸微胶囊粉剂中壬基酚的液相色谱-电喷雾质谱（LC-ESI-MS/MS）检测方法。样品经环己烷∶乙酸乙酯（1∶1,v/v）提取,低温冷冻离心净化,液相色谱-电喷雾质谱测定,内标法定量。通过正交实验优化了样品提取条件,最佳提取条件为提取次数为1次、超声15 min、称样质量为1.5 g,涡旋时间20 s。检出限为0.3μg/kg,线性范围1¹50 ng/m L（r=0.9998）,样品测定结果为36.21¹23.98μg/kg,样品回收率为94.6%¹08.1%,RSD=3.9%¹4.3%（n=6）。该法简便快捷、结果准确,可用于多不饱和脂肪酸微胶囊粉剂中壬基酚的分析测定。 

Determination of Nonylphenol in polyunsaturated fatty acids microencapsulated powder by liquid chromatography tandem mass spectrometry

A sensitive liquid chromatography- tandem mass spectrometry method( LC- MS / MS) was developed for the determination of Nonylphenol( NP) in polyunsaturated fatty acids microencapsulated powder.The Nonylphenol in samples was extracted with the mixture of cyclohexane and ethyl acetate( 1 ∶ 1,v / v).The extractions were purified by centrifuge with low temperature and LC- MS / MS analysis was performed by positive ion electrospray ionization applying multiple reaction monitoring with internal standard method for quantitative analysis.The condition of the sample extraction was optimized by the orthogonal experiment.The optimized fermentation conditions were found to be: extraction 1 time,ultrasonic time 15 min,1.5 g samples and vortex time 20 s.The limits of quantitation( LOQ) was 0.3 μg /kg,and the method showed good linearity between 1~150 ng /m L( r = 0.9998).The results of the samples were 36.21~123.98 μg / kg.The recoveries were between 94.6% to 108.1% and RSD were between 3.9% to14.3%.The method was simple,quick and accurate.The method was proved to be appliable in the determination of NP in polyunsaturated fatty acids microencapsulated powder.