日化香精中甲醛含量的超高效液相色谱分析

Determination of formaldehyde in fragrance for household and personal products by ultra- high performance liquid chromatography

建立了一种测定日化香精中甲醛含量的超高效液相色谱(UPLC)分析方法。香精中的甲醛以2,4-二硝基苯肼作为衍生化试剂进行反应后,直接用UPLC进行分析。采用Agilent ZORBAX Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm,1.8μm)分离;以水-乙腈溶液(体积比为60∶40)为流动相进行等梯度洗脱,流速为0.3 m L/min;检测波长为352 nm,外标法定量。甲醛在0.1~10 mg/L范围内具有良好的线性,检出限为0.03 mg/L,加标回收率为96.3%~104.1%,RSD为0.2%~1.4%(n=3)。将该方法应用于10批日化香精中甲醛含量的测定,结果检出5批日化香精中含有甲醛,但其含量远低于《化妆品卫生规范》中甲醛的使用限量。

An ultrahigh performance liquid chromatography （UPLC） method was established for determination of formaldehyde in fragrance for household and personal products. After derived with 2,4 - dinitrophenyl hydrazine （DNPH） , the formaldehyde in the fragrance was determined by UPLC. The separation was performed on an Agilent ZORBAX Eclipse Plus Cls column （2. 1 mm × 100 mm, 1.8 μm）. The mobile phase was consisted of acetonitrile and water （ volume ratio of 60： 40） with a flow rate of 0. 3 mL/min. The wavelength of UV detector was set at 352 nm. A good linearity of formaldehyde in the range of 0. 1 - 10 mg/L is obtained and the detection limit is about 0. 03 mg/L. The spiked recoveries are ranged within 96.3% 104. 1% ,with relative standard deviations of 0. 2% - 1.4% （n = 3）. 10 batches of fragrance for household and personal products were determined using the established method and five batches are found containing formaldehyde. However, the content of formaldehyde in the samples is much lower than the limit specified by Hygienic Standard for Cosmetics.