齐鲁师范学院学报
齊魯師範學院學報
제로사범학원학보
JOURNAL OF SHANDONG EDUCATION INSTITUTE
2012年
5期
73-76
,共4页
申中兰%郗丹%盛建伟%鞠香%田其燕%孙立臻%张卉
申中蘭%郗丹%盛建偉%鞠香%田其燕%孫立臻%張卉
신중란%치단%성건위%국향%전기연%손립진%장훼
气相色谱-串联质谱法%固相萃取%酱油%三氯丙醇
氣相色譜-串聯質譜法%固相萃取%醬油%三氯丙醇
기상색보-천련질보법%고상췌취%장유%삼록병순
GC-QqQ-MS/MS%SPE%Soy Sauces%3-MCPD
建立了快速、高效的酱油中三氯丙醇的固相萃取净化-气相色谱-串联质谱法(GC—QqQ—MS/MS)测定方法。0.5g酱油,加0.5mL饱和NaCl盐析,超声15min后经弗罗里硅土固相萃取柱净化,无水乙醚洗脱,d,-3-MCPD为内标,七氟丁酰基咪唑衍生化,加饱和NaCl3mL混匀,有机层进GC—QqQ—MS/MS分析。净化时间少于20min。方法回收率为101.36%,线性范围在0.05-5.0mg/ks,线性相关系数R2=O.99997,方法检出限为0.005mg/kg,该方法对酱油中三氯丙醇的测定有良好的效果。
建立瞭快速、高效的醬油中三氯丙醇的固相萃取淨化-氣相色譜-串聯質譜法(GC—QqQ—MS/MS)測定方法。0.5g醬油,加0.5mL飽和NaCl鹽析,超聲15min後經弗囉裏硅土固相萃取柱淨化,無水乙醚洗脫,d,-3-MCPD為內標,七氟丁酰基咪唑衍生化,加飽和NaCl3mL混勻,有機層進GC—QqQ—MS/MS分析。淨化時間少于20min。方法迴收率為101.36%,線性範圍在0.05-5.0mg/ks,線性相關繫數R2=O.99997,方法檢齣限為0.005mg/kg,該方法對醬油中三氯丙醇的測定有良好的效果。
건립료쾌속、고효적장유중삼록병순적고상췌취정화-기상색보-천련질보법(GC—QqQ—MS/MS)측정방법。0.5g장유,가0.5mL포화NaCl염석,초성15min후경불라리규토고상췌취주정화,무수을미세탈,d,-3-MCPD위내표,칠불정선기미서연생화,가포화NaCl3mL혼균,유궤층진GC—QqQ—MS/MS분석。정화시간소우20min。방법회수솔위101.36%,선성범위재0.05-5.0mg/ks,선성상관계수R2=O.99997,방법검출한위0.005mg/kg,해방법대장유중삼록병순적측정유량호적효과。
A fast, effective method for analysis of 3 -MCPD in soy sauces was developed by modified SPE- GC -QqQ- MS/MS method. 0. 5g of soy sauces, which was added 0. 5 mL saturated NaC1, and was extracted by ultrasonic for 15rain, and then was purified by Florisil -SPE. D5 -3 -MCPD and N - Heptafluorobutyrylimidazole was used as the internal standard and derivative reagent respectively The re- covery was 101.36% ,liner ranges were 0.05 -5.0mg/kg,correlation coefficient R2 =0. 99997 ,the limit of detection was O. 005mg/kg. This method meet the requirement of determiantion of 3 - MCPD in soy sauces.