MSPD-GC-MS同时测定酱油及调味液中多组分氯丙醇  

Determination of dichloropanols and monochloropanediols in soy sauce by MSPD-GC-MS using stable isotope dilution technique

作　　者：马金波[1] 张琦[1] 栾燕[1] 迂君[1] 杨丽丽[2] 

机构地区：[1]沈阳市疾病预防控制中心,沈阳110031 [2]沈阳市东陵区疾病预防控制中心,沈阳110015

出　　处：《中国卫生检验杂志》2007年第4期583-585,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的:建立一种快速测定酱油及调味液中多组分氯丙醇的GC-MS测定方法。方法:在样品中加入两种稳定性氘代同位素内标后,样品经过基质固相分散萃取(MSPD)提取与净化,用全扫描定性,选择离子(SIM)定量。结果:各个氯丙醇在进样量在20～400 pg范围内线性良好(r>0.999),3-氯-1,2-丙二醇(3-MCPD)、1,3-二氯丙醇(1,3-DCP)和2,3-二氯丙醇(2,3-DCP)的定量限分别为0.003、0.005和0.005 mg/kg;2种浓度水平下加标重复测定6次,回收率为95%～120%,精密度<10%。结论:方法具有较高的灵敏度、准确度、精密度和特异性,满足了样品中痕量氯丙醇的分析要求。Objective ：To develop a method to determine chloropropanols quickly in soy sauce by GC -MS using stable isotope dilution technique. Methods： Sample was spiked with deuterium - labeled isotope internal standards （ IS）, extracted by matrix solid - phase dispersion （MSPD） and determined by selective ion measure （SIM） mode. Results：A good linear relationship （ r 〉 0. 999） between the amount and area ratio of chloropropanols was obtained over the concentration range of 20 -400 pg. Limits of quantitation （LOQ） of 3 - chlom - 1,2 - propanediol （ 3 - MCPD） and dichlompmpanols （ 1,3 - DCP, 2,3 - DCP） were 0. 003, 0. 005 and 0. 005 mg/kg, respectively. The recoveries of 3 - MCPD, 1,3 - DCP and 2,3 - DCP were 95% ～ 120% （ n = 6） for the soy sauces spiked at two different levels, respectively. RSD 〈 10%. Conclusion：The simultaneous separation and determination of 3 chlompropanols in soy sauce with two kinds of stable isotopes as internal standard are developed with satisfactory sensitivity, accuracy, precision and specificity.

关 键 词：基质固相分散萃取(MSPD) 气相色谱-质谱联用(GC/MS) 氯丙醇 酱油 

分 类 号：O657.63[理学—分析化学]