气相色谱-质谱联用法测定香水类化妆品中的甲醇  

Determination of methanol in perfume cosmetics by GC-MS

作　　者：翟宇 尚博扬 黄青[2] ZHAI Yu;SHANG Bo-yang;HUANG Qing(Ningxia Institute for Drug Control and Research, Yinchuan, Ningxia 750004, China)

机构地区：[1]宁夏回族自治区药品检验研究院,宁夏银川750004 [2]宁夏医科大学,宁夏银川750004

出　　处：《中国卫生检验杂志》2019年第14期1678-1679,1682,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立测定香水类化妆品中甲醇的气相色谱-质谱联用法。方法采用Agilent DB-WAX毛细管色谱柱(30 m×0. 25 mm,0. 25μm),程序升温法,即初始温度为50℃,保持5 min,以15℃/min的速率升温至200℃,保持3 min,选择离子监测模式,用甲醇的保留时间和特征离子定性,外标法峰面积定量,定量离子m/z 31,参考离子m/z 32和29。样品加无水乙醇溶解、定容,涡旋混匀,静置,经0. 22μm有机滤膜过滤,采用气相色谱-质谱联用法测定。结果被测物甲醇与乙醇在本实验条件下能得到很好分离,甲醇在5μg/ml^200μg/ml线性良好(r=0. 999 9),检出限为11. 7 mg/kg,回收率为91. 3%~96. 5%,RSD为2. 6%~3. 1%。结论本法样品前处理简单,分析快速,专属性强,灵敏度高,结果准确可靠,适用于香水类化妆品中甲醇的测定。Objective To establish a GC-MS method for the determination of methanol in perfume cosmetics. Methods The chromatographic column was Agilent DB-WAX( 30 m × 0. 25 mm,0. 25 μm) and programmed temperature was used. The initial temperature was 50 ℃ for 5 min,and the temperature was raised to 200 ℃ at a rate of 15 ℃/min for 3 min. Selective ion monitoring was adopted,the retention time and characteristic ions of methanol were used for qualitative analysis,and external standard method was used for quantitative analysis. The quantitative ion was m/z 31,and reference ions were m/z 32 and m/z29. The sample was dissolved in absolute ethanol,made up to volume,vortexed,and allowed to stand. It was filtered through a 0. 22 μm organic filter membrane and determined by GC-MS. Results The methanol and ethanol can be well separated under the experimental conditions. The calibration curves of methanol in the range of 5 μg/ml-200 μg/ml( r = 0. 999 9)showed good linearity,the detection limit was 11. 7 mg/kg,and the average recoveries were within 91. 3%-96. 5%,with relative standard deviations of 2. 6%-3. 1%. Conclusion The method is simple,rapid,sensitive and specific,and the result is accurate and reliable. It is suitable for the determination of methanol in perfume cosmetics.

关 键 词：甲醇 香水 气相色谱-质谱联用法 化妆品 

分 类 号：O657.71[理学—分析化学]