分析测试学报2011,Vol.30Issue(6):665-669,5.DOI:10.3969/j.issn.1004-4957.2001.06.014
高效液相色谱-串联质谱法测定调味料中的痕量苯甲酸与山梨酸
Determination of Benzoic Acid and Sorbic Acid in Seasoning by High Performance Liquid Chromatography- Tandem Mass Spectrometry
摘要
Abstract
A high performance liquid chromatography- tandem mass spectrometric (HPLC -MS/MS) method was developed for the determination of benzoic acid and sorbic acid in seasoning. The samples of seasoning were acidified by hydrochloric acid and extracted by diethyl ether for several times. The extract was washed with acidic sodium chloride, then evaporated to dryness. The residue was filtrated with membrane and reserved for analysis after dissolved in 1 mL 90% 0. 2 mmol/L NH4OAc( pH 5.0) acetonitrile solution. The conditions of extraction and purification were optimized. The analyte was identified under negative electrospray ionization ( ESI - ) mode and analyzed quantitatively by the external standard method under the single reaction monitoring(SRM) mode. The calibration curve showed a good linearity in the concentration range of 0. 5 - 5 mg/L with correlation coefficients (r2 ) more than 0. 995. The limits of detection (LODs) of benzoic acid and sorbic acid beth were 0. 1 mg/kg and their limits of quantitation(LOQs) were 0. 4 mg/kg and 0. 5 mg/kg, respectively. The recoveries of benzoic acid and sorbic acid were in the ranges of 84% -98% and 82% -96% , respectively, with RSDs less than 3%. Actual test results also showed that the method was simple, sensitive and accurate, and was suitable for the trace determination of benzoic acid and sorbic acid residue in complex matrices.关键词
高效液相色谱-质谱联用/痕量检测/苯甲酸/山梨酸/调味料Key words
HPLC - MS/MS/ trace detection/ benzoic acid/ sorbic acid/ seasoning分类
化学化工引用本文复制引用
王祖翔,任连兵,蒋俊,周洪斌,李平,吕平,万荣..高效液相色谱-串联质谱法测定调味料中的痕量苯甲酸与山梨酸[J].分析测试学报,2011,30(6):665-669,5.基金项目
食品中几类掺假非蛋白氮检测技术研究(2009KJ35) (2009KJ35)