Simultaneous determination of Cr(Ⅲ) and Cr(Ⅵ) in printing ink by HPLC-ICP-MS
MENG Nian, YE Yuzeng, LIU Fangying
Bauhinia Variegata Ink & Chemicals (Zhongshan) Company Limited, Zhongshan 528459, China
摘要：建立以NH4NO3为流动相，高效液相色谱-电感耦合等离子体质谱联用（HPLC-ICP-MS）技术测定印刷油墨中可迁移的Cr（Ⅲ）和Cr（Ⅵ）的方法。样品以0.07 mol/L的pH 1.1～1.3盐酸溶液为萃取剂，于(937±2)℃水浴振荡萃取1 h，然后静置1 h，用0.45 μm过滤头过滤后取1.0 mL滤液，加入1.0 mL 0.07 mol/L氨水及8.0 mL缓冲液在50℃水浴中静置50 min，取出样品溶液，冷却至室温后用HPLC-ICP-MS仪分析测试。Cr（Ⅲ）和Cr（Ⅵ）的质量浓度在0.04～0.20 μg/L范围内与色谱峰面积呈良好的线性关系，线性相关系数分别为0.999 1和0.999 8，方法检出限分别为0.007 mg/kg和0.002 mg/kg。加标回收率为88.2%～114.6%，Cr（Ⅲ）和Cr（Ⅵ）测定结果的相对标准偏差分别为2.7%和3.5%（n=10）。该方法快速、准确，适用于测定基体复杂的油墨中可迁移Cr（Ⅲ）和Cr（Ⅵ）。
Abstract：A method for the determination of migratory Cr(Ⅲ) and Cr(Ⅵ) in printing ink by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) with NH4NO3 as the mobile phase was established. The samples were extracted with 0.07 mol/L hydrochloric acid solution(pH 1.1-1.3) for 1 h by water bath oscillation extraction at (37±2)℃, then stayed for 1 h and filtered with a membrane filter(0.45 μm), 1.0 mL ammonia water and 8.0 mL buffer solution were adding to 1.0 mL migration solution and placed in a 50℃water bath to stayed for 50 min, and the mixture solution was taken out and cooled to room temperature, and analyzed by HPLC-ICP-MS. The mass concentration of Cr(Ⅲ) and Cr(Ⅵ) had good linear relationship with the chromatographic peak area in the range of 0.04-0.20 μg/L, The linear correlation coefficients of Cr(Ⅲ) and Cr(Ⅵ) were 0.999 1 and 0.999 8, respectively. The detection limits of Cr(Ⅲ) and Cr(Ⅵ) were 0.007, 0.002 mg/kg, respectively. The recoveries ranged from 88.2% to 114.6%. The relative standard deviations of Cr(Ⅲ) and Cr(Ⅵ) determination results were 2.7% and 3.5%(n=10), respectively. The method is fast and accurate, which is suitable for determining the migration of Cr(Ⅲ) and Cr(Ⅵ) in a complex matrix ink.
Keywords：HPLC-ICP-MS; printing ink; Cr(Ⅲ); Cr(Ⅵ)
蒙念，叶羽增，刘芳英. HPLC-ICP-MS法检测印刷油墨中可迁移Cr(Ⅲ)和Cr(Ⅵ)[J].化学分析计量，2019，28(5)：19-23. MENG N，YE Y Z，LIU F Y. Simultaneous determination of Cr(Ⅲ) and Cr(Ⅵ) in printing ink by HPLC-ICP-MS[J]. Chemical analysis and meterage，2019，28(5)：19-23.