摘要
采用多同位素内标法,结合七氟丁酰基咪唑(HFBI)衍生化的气相色谱-质谱(GC—MS)联用技术,建立了食品中4种氯丙醇含量的检测方法。对比了不同来源HFBI衍生试剂的作用性能,对定量内标物和校正标准的选择进行了比较。结果表明:仅用2种同位素内标(3.氯-1,2.丙二醇-d5(或2.氯.1,3.丙二醇.d,)和1,3.二氯.2.丙醇-d5)校正,同样可达到准确测定食品中4种氯丙醇含量的要求;若采用3-氯-1,2-丙二醇(3-MCPD)为标准物定量测定2-氯-1,3-丙二醇(2-MCPD)时,所得2-MCPD结果偏低,仅为以2.MCPD为标准物定量结果(真实值)的52.1%-77.8%。在最佳条件下进行了方法学指标的系统验证。4种氯丙醇的最低检出限为2.5~10gg/kg:在100-2000ng范围内,氯丙醇与内标物峰面积的比值和质量呈线性关系俾z〉0.9990)。以酱油和方便面调料粉为基质,进行100、200、4001xg/kg-1.个水平的加标回收实验,4种氯丙醇的回收率均值为90.1%~107%,相对标准偏差(RSD)为3.37%~10.4%(n=6),均满足痕量分析的要求。
An analytical method was developed to determine 4 kinds of chloropropanols in foods using gas chromatography mass spectrometer coupled with the multi-isotopic internal standard technique. The performance difference between different brands of HFBI as a derivativization reagent and internal standard selection for quantification were discussed. Under the optimal conditions, the limits of detection (LOD) were 2.5-10 gg/kg for 4 kinds of chloropropanols. According to the internal standard calibration, an excellent linearity between 100 ng and 2000 ng of chloropropanols (R2 〉 0.9990) was obtained. When chloropropanols were spiked at levels of 100, 200, 400 mg/kg in soy sauce and seasoning powder of instant noodles, the average recovery rates were 90.1%-107%, with relative standard deviation (RSD) of 3.37%-10.4% (n = 6). The application of only 2 kinds of internal standards (chloropropane-l,2-diol-d5 or 2-chloropropane-l,3-diol-d5 and 1,3-dichloro-2-propanol-ds) can reveal accurate and precise determination for 4 kinds of chloropropanols. When 3-chloropropane-l,2-diol (3-MCPD) was used to calibrate 2-MCPD in foods, the level of 2-chloropropane-1,3-diol (2-MCPD) was only 52.1%-77.8% of the real content.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2013年第18期131-136,共6页
Food Science
基金
国家自然科学基金面上项目(81172671)
卫生部公益性行业科研专项(200902009)
福建省杰出青年基金项目(2011J06011)
福建省医学创新课题(2011-CX-21)
关键词
食品
氯丙醇
基质分散固相萃取法
同位素稀释技术
气相色谱-质谱法
food
chloropropanoh dispersion matrix solid-phase extraction
isotopic internal standard technique
gaschromatography-mass spectrometer (GC-MS)