超高效液相色谱-串联质谱法同时测定调味料中的17种防腐剂和抗氧化剂  

Simultaneous determination of 17 preservatives and antioxidants in condiments using ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

作　　者：凌云[1,2] 储晓刚[2] 张峰[2] 陈琦[2,3] 赵云峰[1] 吴永宁[1] 张晨光[1] 

机构地区：[1]中国疾病预防控制中心,北京100021 [2]中国检验检疫科学研究院,北京100123 [3]陕西科技大学,陕西西安710021

出　　处：《色谱》2011年第8期723-730,共8页Chinese Journal of Chromatography

基　　金：北京市科技计划项目(D08050200310804;D08050200310803);财政部质检公益性行业科研项目(200910145);国家科技支撑计划课题(2009BADB9B02)

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定调味料中11种防腐剂和6种抗氧化剂的定性、定量分析方法。低脂肪和中等脂肪含量的调味料样品用饱和NaCl水溶液(用磷酸调pH为2～3)稀释混合均匀,然后用乙腈提取,正己烷液-液萃取净化(中等脂肪含量的样品提取液还需经C8固相萃取柱进一步的净化处理);脂肪含量高的样品先用正己烷稀释,再用饱和NaCl水溶液(用磷酸调pH为2～3)溶解样品,然后用乙腈提取,提取液进一步经C8固相萃取柱净化处理。提取液经C18反相色谱柱(150mm×2.1mm,1.7μm)分离,流动相为20mmol/L乙酸铵水溶液和乙腈,梯度洗脱,以电喷雾离子源负离子多反应监测(MRM)模式进行MS/MS检测。17种分析物在线性范围内具有较好的线性关系,相关系数r≥0.9955,其定量限(LOQ,信噪比为10)为0.05～5mg/kg;空白样品中的添加回收率为79.7%～118%,精密度(以相对标准偏差计)为0.57%～13.1%。该方法适用于调味品中防腐剂和抗氧化剂的检测。An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry（UPLC-ESI-MS/MS） method was developed for the simultaneous determination of 11 preservatives and 6 antioxidants in condiments.The condiment sample with low fat or middle fat was diluted with saturated NaCl solution（adjusting pH to 2-3 with phosphoric acid）,then extracted with acetonitrile.The extract was purified using liquid-liquid extraction with hexane,and the sample with middle fat was further purified using solid phase extraction with a C8 column.The condiment sample with high fat was diluted with hexane,then dissolved with saturated NaCl solution（adjusting pH to 2-3 with phosphoric acid）,and extracted with acetonitrile.The extract was purified using solid phase extraction with a C8 column.The analysis was performed on a C18 column（150 mm×2.1 mm,1.7 μm） using a gradient elution with the mobile phases of 20 mmol/L ammonium acetate buffer and acetonitrile,and determined by tandem mass spectrometry in negtive ESI mode under multiple reaction monitoring（MRM） mode.The method had good linearity（r≥0.995 5）.The limits of quantification（LOQs）（S/N=10） of 17 analytes ranged from 0.05 mg/kg to 5 mg/kg.The recoveries ranged from 79.7% to 118% at three spiked levels,the relative standard deviations（RSDs） ranged from 0.57% to 13.1%.The method can be applied for the determination of preservatives and antioxidants in condiments.

关 键 词：固相萃取 超高效液相色谱-串联质谱 防腐剂 抗氧化剂 调味料 

分 类 号：O658[理学—分析化学]