高效液相色谱-电感耦合等离子体质谱法测定化妆品中2-溴-2-硝基-1,3-丙二醇

Determination of 2-Bromo-2-nitro-1,3-propanediol in Cosmetics by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)测定化妆品中2-溴-2-硝基-1,3-丙二醇的方法。采用ZORBAX RX-C_8色谱柱(150×2.1 mm,5μm)进行分离,以甲醇-水-5%磷酸(10∶985∶5,用2 mol/L NaOH调至pH 3.0)为流动相,流速为0.7 m L/min,柱温为室温。结果显示,2-溴-2-硝基-1,3-丙二醇在2.5 min处出峰,其线性范围为0.01~1.0 mg/L,相关系数为0.999 9。不同基质化妆品的方法检出限均为1.0μg/g,回收率为94.6%~101.3%,相对标准偏差(RSD,n=6)为1.5%~4.5%。该方法快速、准确、灵敏、无干扰,适用于化妆品中2-溴-2-硝基-1,3-丙二醇的定性定量测定。

A new method was established to determine 2-bromo-2-nitro-1,3-propanediol in cosmetics by high performance liquid chromatography-inductively coupled plasma mass spectrometry（HPLC-ICP-MS）. The analyte was separated on a ZORBAX-C8 column （150×2.1 mm, 5 μm） using methanol-water-5% phosphoric acid （10 ∶ 985 ∶ 5, pH value was adjusted to 3.0 with 2 mol/L NaOH） as mobile phase. The flow rate was set at 0.7 mL/min. The column temperature was room temperature. The results indicated that the calibration curve of 2-bromo-2-nitro-1,3-propanediol was linear in the range of 0.01-1.0 mg/L,with a correlation coefficient（r） of 0.999 9. The detection limits of different matrix samples were all 1.0 μg/g. The spiked recoveries of 2-bromo-2-nitro-1,3-propanediol ranged from 94.6% to 101.3%, with RSDs（n=6） of 1.5%- 4.5%. The method showed the advantages of rapidness,sensitivity,accuracy and little interference,and it could be used for the qualitative and quantitative determination of 2-bromo-2-nitro-1,3-propanediol in cosmetics.