固相萃取-凝胶渗透色谱净化-气相色谱-质谱法测定番茄红素软胶囊中6种对羟基苯甲酸酯类防腐剂  

Determination of 6 para-hydroxybenzoic acid esters in health food lycopene soft capsule by solid phase extraction-gel permeation chromatography purification-gas chromatography-mass spectrometry

作　　者：刘运明[1] 周长美[1] 姜新[1] 

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009

出　　处：《中国卫生检验杂志》2015年第20期3471-3474,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立固相萃取、凝胶渗透色谱净化样品,气相色谱-质谱法同时测定番茄红素软胶囊中6种对羟基苯甲酸酯类防腐剂的分析方法。方法样品用丙酮-乙酸乙酯(1∶1,V/V)提取,提取液用Pro Elut TPC固相萃取柱去除番茄红素,再用凝胶渗透色谱(GPC)去除样品中的油脂后,用气相色谱-质谱法测定,基质匹配标准溶液以外标法定量。结果当质量浓度为0.05μg/ml^1.0μg/ml时,各种防腐剂的线性关系良好,相关系数(r)均>0.999,检出限为0.03μg/g^0.05μg/g,定量限为0.09μg/g^0.15μg/g,在0.2μg/g、0.5μg/g、1.0μg/g 3种添加水平下,样品加标回收试验的平均回收率为81%~96%,相对标准偏差(RSD)为4.2%~8.5%。结论该方法灵敏度高、选择性好、抗干扰性强,定性、定量准确,可满足同时测定基质复杂样品中多种对羟基苯甲酸酯类防腐剂的检测要求。Objective To establish a method for the simultaneous detection of 6 para-hydroxybenzoic acid esters preservatives in health food lycopene soft capsule by GC-MS after solid-phase extraction（ SPE） and cleaned-up with gel permeation chromatography（ GPC）. Methods Samples were extracted with acetone-ethyl acetate（ 1∶1,V / V）,and then remove the lycopene in the extract with Pro Elut TPC solid-phase extraction column and removed the grease by gel permeation chromatography（ GPC） and determined by GC-MS. The target analytes were separated and detected by the GC-MS. The matrix-matched standard solution were quantified by external standard method. Results When the matrix quantity was in the range of 0. 05 μg / ml-1. 0 μg / ml;the linear relationship was good and the correlation coefficients（ r） of the every para-hydroxybenzoic acid esters were larger than 0. 999; the detection limits were in 0. 03 μg / g-0. 05 μg / g; the quantitative limit was in 0. 09 μg / g-0. 15 μg / g; At three additive levels of 0. 2 μg / g,0. 5 μg / g and 1 μg / g,the average recovery rate of additive samples with recovery test was among 81%-96%; the RSD was among 4. 2%-8. 5%. Conclusion This method has high sensitivity,good selectivity and strong anti-interference ability,and it can meet the simultaneous determination of many kinds of matrix complex samples for the detection of hydroxylbenzoic acid ester preservatives.

关 键 词：固相萃取 凝胶渗透色谱 气相色谱-质谱法 对羟基苯甲酸酯类防腐剂 番茄红素软胶囊 

分 类 号：O657.63[理学—分析化学]