食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2013年
2期
444-450
,共7页
罗冠中*%谭亚军%孟云彩
囉冠中*%譚亞軍%孟雲綵
라관중*%담아군%맹운채
婴幼儿配方乳粉%酚类化合物%环境激素%测定
嬰幼兒配方乳粉%酚類化閤物%環境激素%測定
영유인배방유분%분류화합물%배경격소%측정
infant formulas%phenolic compounds%environmental hormones%determination
目的建立婴幼儿配方乳粉中双酚 A(BPA)、双酚 F(BPF)、己烷雌酚、己烯雌酚、双烯雌酚、辛基酚、壬基酚7种酚类环境激素的液相色谱-串联四极杆质谱检测方法.方法以1%三氯乙酸和乙腈提取, HLB 固相萃取净化,由 C18液相色谱柱分离,以电喷雾离子源负离子模式,多反应监测(MRM)条件下对7种物质进行检测,基质加标标准曲线法定量.结果7种化合物检出限在0.5~5μg/kg,定量限从1.5~15μg/kg.7种物质从定量限到50 ng/mL 范围内线性关系良好.在三水平加标回收试验中,7种化合物的回收率在73.5%~97.9%之间, RSD 为5.6%~13.6%.结论本文对7种环境激素同时检测的方法具有准确、高效、灵敏、特异性强等优点,为食品安全风险监控方法提供参考依据.
目的建立嬰幼兒配方乳粉中雙酚 A(BPA)、雙酚 F(BPF)、己烷雌酚、己烯雌酚、雙烯雌酚、辛基酚、壬基酚7種酚類環境激素的液相色譜-串聯四極桿質譜檢測方法.方法以1%三氯乙痠和乙腈提取, HLB 固相萃取淨化,由 C18液相色譜柱分離,以電噴霧離子源負離子模式,多反應鑑測(MRM)條件下對7種物質進行檢測,基質加標標準麯線法定量.結果7種化閤物檢齣限在0.5~5μg/kg,定量限從1.5~15μg/kg.7種物質從定量限到50 ng/mL 範圍內線性關繫良好.在三水平加標迴收試驗中,7種化閤物的迴收率在73.5%~97.9%之間, RSD 為5.6%~13.6%.結論本文對7種環境激素同時檢測的方法具有準確、高效、靈敏、特異性彊等優點,為食品安全風險鑑控方法提供參攷依據.
목적건립영유인배방유분중쌍분 A(BPA)、쌍분 F(BPF)、기완자분、기희자분、쌍희자분、신기분、임기분7충분류배경격소적액상색보-천련사겁간질보검측방법.방법이1%삼록을산화을정제취, HLB 고상췌취정화,유 C18액상색보주분리,이전분무리자원부리자모식,다반응감측(MRM)조건하대7충물질진행검측,기질가표표준곡선법정량.결과7충화합물검출한재0.5~5μg/kg,정량한종1.5~15μg/kg.7충물질종정량한도50 ng/mL 범위내선성관계량호.재삼수평가표회수시험중,7충화합물적회수솔재73.5%~97.9%지간, RSD 위5.6%~13.6%.결론본문대7충배경격소동시검측적방법구유준학、고효、령민、특이성강등우점,위식품안전풍험감공방법제공삼고의거.
@@@@Objective To establish an analytical method for determination of 7 phenolic environmental hormones-Bisphenol A, Bisphenol F, Hexestrol, Diethylstilbestrol, Dienestrol, Octylphenol, and Nonylphenol in infant formulas by liquid chromatography-triple quadrupole mass spectrometry. Methods Samples were extracted with 1% trichloroacetic acid and acetonitrile and purified by HLB solid phase extraction (SPE). The 7 compounds were separated by C18 column and analyzed by LC-MS/MS under multiple reaction monitoring (MRM) mode via negative electrospray ionization, and qualified by curvilinear equations of spiking standard in matrix. Results The limits of determination (LOD) of 7 compounds were 0.5~5 μg/kg, and the limits of quan-titation were 1.5~15 μg/kg. The results showed a good linearity over the range of LOQ to 50 ng/mL. The aver-age recoveries of 7 compounds were from 73.5% to 97.9% with the relative standard deviations (RSDs) of 5.6%~13.6% by three-level spiking tests. Conclusion The reported method of analyzing 7 environmental hormones simultaneously has the advantages of accuracy, efficiency, sensitivity and specificity, which will pro-vide references for the risk monitoring of food safety.