色谱2011，Vol.29Issue(8)：723-730,8.DOI:10.3724/SP.J.1123.2011.00723
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
摘要
Abstract
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 CR column. The analysis was performed on a C18 column (150 mm x 2. I mm ,1.7 |xm) 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Key words
solid phase extraction (SPE)/ ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/ preservatives/ antioxidants/ condiments分类
化学引用本文复制引用
凌云,储晓刚,张峰,陈琦,赵云峰,吴永宁,张晨光..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[J].色谱,2011,29(8):723-730,8.基金项目
北京市科技计划项日(D08050200310804,D08050200310803)、财政部质检公益性行业科研项日(200910145)和国家科技支撑计划课题(2009BADB9B02) （D08050200310804,D08050200310803）
