气相色谱-质谱法同时测定果蔬清洗剂中12种防腐剂和抗氧化剂

建立了气相色谱-质谱同时检测果蔬清洗剂中12种防腐剂和抗氧化剂的方法。果蔬清洗剂样品先加入乙醇，经旋转蒸发除去样品中的水分，然后用正己烷饱和的乙腈溶液提取，饱和氯化钠溶液洗涤净化，净化后的样品溶液浓缩后用乙腈定容。被测组分经HP-5MS UI石英毛细管色谱柱（30 m×0.25 mm×0.25 μm）分离后在选择离子监测模式下测定。12种防腐剂和抗氧化剂在0.1~10 mg/L范围内线性关系良好，相关系数（r²）>0.999；检出限和定量限分别为0.010~0.030 mg/kg和0.030~0.090 mg/kg。按照建立的方法进行0.2、2.0和10 mg/kg 3个添加水平的加标回收试验，回收率为68.3%~115.3%，相对标准偏差为3.1%~11.3%。该法灵敏度高，定性准确，前处理净化效果好，适用于果蔬清洗剂中防腐剂和抗氧化剂的检测。

Simultaneous determination of 12 preservatives and antioxidants in fruit and vegetable detergents by gas chromatography-mass spectrometry

A method was established for the simultaneous determination of 12 preservatives and antioxidants in fruit and vegetable detergents by gas chromatography-mass spectrometry (GC-MS). First, ethanol was added to remove the water in the sample by rotary evaporation and was extracted with acetonitrile in saturated n-hexane. Finally, the residual surfactant in the sample solution was removed with a saturated sodium chloride solution. The purified sample solution was concentrated and metered volume by acetonitrile. The preservatives and antioxidants were separated on a HP-5MS UI capillary column (30 m×0.25 mm×0.25 μm), and detected in the selective ion monitoring (SIM) mode. The method had a good linearity in the range of 0.1-10 mg/L with correlation coefficients (r²)>0.999, and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.010-0.030 mg/kg and 0.030-0.090 mg/kg, respectively. The recoveries of the 12 preservatives and antioxidants at three spiked levels (0.2, 2.0 and 10 mg/kg) were 68.3%-115.3% with the relative standard deviations (RSDs) of 3.1%-11.3%. (n=7) The method is sensitive and accurate, and can be suitable for the determination of preservatives and antioxidants in fruit and vegetable detergents.