超高效合相色谱-串联质谱法测定口含烟中对羟基苯甲酸酯

Determination of p-Hydroxybenzoic Esters (Parabens) in Snus by UPC2-MS/MS

  • 摘要: 建立了QuEChERS-超高效合相色谱-串联质谱法(UPC2-MS/MS)测定口含烟中对羟基苯甲酸酯类防腐剂。采用乙腈提取,基质分散固相萃取净化,UPC2 TM HSS C18 SB色谱柱(3.0 mm×100 mm×1.8 μm)分离,内标法定量。优化后的对羟基苯甲酸酯的合相色谱分离条件为:主要流动相为CO2,改性剂为甲醇-异丙醇混合溶液(V/V,1∶1),系统流速1.5 mL/min,离子化辅助溶剂(补偿溶剂)为0.1%甲酸-甲醇溶液,动态备压1.03×107 Pa,柱温55 ℃,可在3 min内完成单个样品分析。4种成分的线性范围均为0.5~5.0 mg/kg;在低、中、高加标水平下,方法的平均回收率为94.6%~105.6%,相对标准偏差小于5%。实际样品测定结果表明,单个成分的含量和多种成分的总含量均小于10 mg/kg,低于GB 2760—2014对于此类防腐剂在食品中添加限量的要求。该方法环境友好、高效、准确,适用于口含烟中对羟基苯甲酸酯类物质的测定。

     

    Abstract: An effective analytical method using QuEChERS coupled with ultra-performance convergence chromatography-tandem mass spectrometry (UPC2-MS/MS) for determination of p-hydroxybenzoic esters (parabens) in snus was developed. In the present work, acetonitrile was selected as extraction solvent, extraction kit (25 mg PSA, 7.5 mg Carbon, 150 mg MgSO4) was evaluted to purify samples. The target analytes were separated on UPC2 TM HSS C18 SB (3.0 mm×100 mm×1.8 μm) column, and quantified by internal standard method. The optimal separation conditions on UPC2 were as follows: the main mobile phase was CO2, and modifier was methanol-isopropanol (V/V, 1∶1), the flow rate was 1.5 mL/min, the assistant ionization solvent (compensate solvent) was methanol with 0.1% formic acid, the pressure of automated backpressure regulator (ABPR) was 1.03×107 Pa, and the temperature of column was 55 ℃, the single analysis would complete within 3 min. The calibration curves are linear in the range of 0.5-5.0 mg/kg. The average recoveries of three addition levels are in the range of 94.6%-105.6% with RSD less than 5%. The detection results showed that parabens contents in snus are lower than the limits regulated by national standard GB 2760—2014 (<10 mg/kg). The proposed method is environmental friendly, high efficiency, accurate, which is suitable for analysis of parabens in snus.

     

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