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目的建立测定尿中2,5-己二酮的毛细管气质联用测定法。方法尿样经酸化后,用乙酸乙酯提取,提取液用气相色谱-质谱联用仪进行检测,利用保留时间和化合物特征离子定性,选择离子法定量。结果取样2．0 ml,提取液1．0 ml,进样1．0μl,分流比为10:1,尿中2,5-己二酮的线性范围为0．25-15．00 mg／L;相对标准偏差(RSD)为1．75％～4．99％;加标回收率为92．0％～106．8％;检测限(LOD)为0．028 mg／L;定量限(LOQ)为0．25 mg／L。结论建立的方法灵敏度高,干扰少,可靠性优于气相色谱法,适用于尿中2,5-己二酮含量的测定。
Objective To establish a method for the determination of 2,5-hexanedione in urine by capillary gas chromatography-mass spectrometry. Methods The urine sample was acidified and extracted with ethyl acetate. The extract was detected by gas chromatography - mass spectrometry (GC / MS). The retention time and the characterization of the compound were qualitatively and qualitatively determined by ion - selective method. Results The results showed that the linear range of 2,5-hexanedione in urine was 0.25-15.00 mg / L for 2.0 ml of sample, 1.0 ml of extract and 1.0 μl of injection. The split ratio was 10: 1. ; The relative standard deviation (RSD) was 1.75% ~ 4.99%; the recoveries were 92.0% -106.8%; the limit of detection (LOD) was 0.028 mg / L; ) Is 0.25 mg / L. Conclusion The established method has high sensitivity, less interference and better reliability than GC, which is suitable for the determination of 2,5-hexanedione in urine.