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目的建立高效液相色谱(HPLC)-串联质谱法(MS/MS)测定母乳中六溴环十二烷三种非对映异构体的方法。方法称取3~5 g冻干母乳样品,加入13C-六溴环十二烷内标,索氏提取,提取液晾干后经6 ml环己烷/乙酸乙酯(1∶1)溶解,凝胶渗透色谱(GPC)除脂,收集液旋转蒸发至近干,加入8 ml正己烷溶解,再加入2 ml浓硫酸进一步除脂,静置分层,收集上清液,正己烷萃取3次,将上清液合并,氮吹至干,定容于100μl甲醇,用HPLC-MS/MS测定。结果方法线性范围为1~50μg/L,相关系数0.9997~0.9998,检出限0.12~0.22μg/L;三个水平的平均加标回收率为82.80%~110.60%;日内相对标准偏差为2.72%~9.02%;日间相对标准偏差为3.49%~5.25%。结论该方法用于测定母乳中六溴环十二烷三种非对映异构体,具有操作简单、基质干扰少、准确可靠的优点,可满足检测需求。
Objective To establish a method for the determination of three diastereomers of HBCD in breast milk by high performance liquid chromatography-tandem mass spectrometry (MS / MS). Methods Weigh 3 to 5 g samples of lyophilized breast milk, add 13C-HBCD internal standard and extract from Soxhlet. After the extract is dried, it is dissolved in 6 ml cyclohexane / ethyl acetate (1: 1) Gel filtration chromatography (GPC) degreasing, the collection was rotary evaporation to near dry, add 8 ml of n-hexane dissolved, then add 2 ml of concentrated sulfuric acid further degreasing, standing stratification, the supernatant was collected, n-hexane extraction three times, The supernatants were combined, nitrogen blown to dryness and fixed in 100 [mu] l of methanol, as determined by HPLC-MS / MS. Results The linear range of the method was 1 ~ 50μg / L, the correlation coefficient was 0.9997 ~ 0.9998, the detection limit was 0.12 ~ 0.22μg / L. The average recoveries were 82.80% ~ 110.60% at three levels. The relative standard deviations were 2.72% ~ 9.02%. The relative standard deviations during the day were 3.49% -5.25%. Conclusion The method is suitable for the determination of three diastereomers of HBCD in breast milk. The method has the advantages of simple operation, less matrix interference, accurate and reliable, and can meet the testing needs.