气相色谱-三重四极杆串联质谱法测定油脂类食品中氯丙醇酯
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摘要
建立一种气相色谱-三重四极杆串联质谱(GC-MS/MS)法检测油脂类食品中氯丙醇酯的分析方法。样品提取脂肪后,取脂肪加内标并经甲醇钠水解,氯丙醇酯被水解为游离态的氯丙醇,水解液经酸中和后,用基质分散固相萃取柱净化,乙醚洗脱液脱水浓缩,用七氟丁酰基咪唑进行衍生,GC-MS/MS进样分析。质谱采用多反应监测模式(MRM)分析,2种一氯丙二醇酯,2种二氯丙醇酯,分别使用其相应的氘代标记的氯丙醇酯和氘代标记的二氯丙醇作为定量内标。所有氯丙醇酯衍生物都通过两个独立的MRM离子对进行检测,均在16min内流出,分离良好,线性范围为5~350ng,相关系数r均在0.99以上,低、高二种浓度加标回收率在87.6%~106.4%之间,相对标准偏差在3.28%~8.83%范围,检出限(S/N≥3)为0.002~0.006mg/kg。
An method was established to detect fatty acid esters of chloropropanols in fat-rich samples by gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).The samples were shattered and fat were extracted according to national standards.D5 isotope labeled internal standards were spiked into the extracted fat.The fatty acid esters of chloropropanols in fat was converted into the free(non-esterified)form by alkaline hydrolysis.The solution containing chloropropaneols was cleaned-up with matrix solid phase dispersion(MSPD)extraction.Then,it was derivatized with 1-(heptafluorobutyryl)imidazole(HFBI).The analysis was performed by gas chromatography-triple quadrupole tandem mass spectrometry with multi-reaction mode(MRM).The calibration curves of 4 chloropropaneols were linear(correlatiom coefficient r>0.99)within the range of 5-350 ng.The recoveries ranged from 87.6% to106.4%,with the relative standard deviations ranging from 3.28%to 8.83%.The detection limits were 0.002-0.006 mg/kg.The method is suitable for determining fatty esters of chloropropanediols in fat-rich samples.
An method was established to detect fatty acid esters of chloropropanols in fat-rich samples by gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).The samples were shattered and fat were extracted according to national standards.D5 isotope labeled internal standards were spiked into the extracted fat.The fatty acid esters of chloropropanols in fat was converted into the free(non-esterified)form by alkaline hydrolysis.The solution containing chloropropaneols was cleaned-up with matrix solid phase dispersion(MSPD)extraction.Then,it was derivatized with 1-(heptafluorobutyryl)imidazole(HFBI).The analysis was performed by gas chromatography-triple quadrupole tandem mass spectrometry with multi-reaction mode(MRM).The calibration curves of 4 chloropropaneols were linear(correlatiom coefficient r>0.99)within the range of 5-350 ng.The recoveries ranged from 87.6% to106.4%,with the relative standard deviations ranging from 3.28%to 8.83%.The detection limits were 0.002-0.006 mg/kg.The method is suitable for determining fatty esters of chloropropanediols in fat-rich samples.
引文
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[8]GB/T 5009.6-2003.Determination of Fat in Foods(食品中脂肪的测定).
[9]GB/T 5009.56-2003.Method for Analysis of Hygienic Standard of Pastry(糕点卫生标准分析方法).
[10]GB/T 5413.3-2010.Determination of Fat in Foods for Infantsr and Yound Children Milk and Milk products(婴幼儿食品和乳品中脂肪的测定).
[11]European Commission Decision,2002/657/EC,Implementing Council Directive96/23/EC Concerning the Performance of Analytical Methods and the Interpretation of Results,Offic J Eur Commun.L221(2002)8.
[2]FU W S,WU S M,HUA J,et al.Chinese Journal of Analytical Chemistry(傅武胜,吴少明,华娟,等.分析化学),2014,42(4):469.
[3]LIU Q,HAN F,XIE K,et al.J Chromatogr A,2013,1314:208.
[4]YAN X B,WU S M,LI N,et al.Chinese Journal of Chromatography.(严小波,吴少明,里南,等.色谱),2013,31(2):95.
[5]Dubois M,Tarres A,Goldmann T,et al.J Chromatogr A,2012,1236:189.
[6]Haines T D,Adlaf K J,Pierceall R M,et al.J Ameri Oil Chem Soci,2011,88:1.
[7]Li He-li,Chen Da-wei,Miao Hong,et al.J Chromatogr A,2015,1410:99.
[8]GB/T 5009.6-2003.Determination of Fat in Foods(食品中脂肪的测定).
[9]GB/T 5009.56-2003.Method for Analysis of Hygienic Standard of Pastry(糕点卫生标准分析方法).
[10]GB/T 5413.3-2010.Determination of Fat in Foods for Infantsr and Yound Children Milk and Milk products(婴幼儿食品和乳品中脂肪的测定).
[11]European Commission Decision,2002/657/EC,Implementing Council Directive96/23/EC Concerning the Performance of Analytical Methods and the Interpretation of Results,Offic J Eur Commun.L221(2002)8.