江西农业学报
江西農業學報
강서농업학보
ACTA AGRICULTURAE JIANGXI
2013年
7期
94-97,101
,共5页
张建莹%沈金灿%岳振峰%吴卫东%罗耀
張建瑩%瀋金燦%嶽振峰%吳衛東%囉耀
장건형%침금찬%악진봉%오위동%라요
液相色谱-质谱%牛奶%光引发剂%残留
液相色譜-質譜%牛奶%光引髮劑%殘留
액상색보-질보%우내%광인발제%잔류
LC-TMS%Milk%Photoinitiator%Residue
建立了牛奶中11种光引发剂残留的定性和定量测定分析方法。样品经Carrez试剂沉淀蛋白质后,使用乙腈提取,HLB固相萃取柱净化,乙腈洗脱,洗脱液用氮气吹干后用50%乙腈水溶液定容,采用液相色谱-串联质谱进行测定。分析物采用电喷雾电离,正离子扫描,多反应监测(MRM)模式检测,其中7种光引发剂使用内标法定量,4种光引发剂使用外标法定量。11种光引发剂在5.00~200μg/L浓度范围内线性关系良好,相关系数均大于0.990。11种光引发剂的测定低限均为1.0μg/kg。在添加浓度1.00~100μg/kg范围内,加标回收率为74.3%~112%,相对标准偏差为0.57%~16.3%。本方法简便、有效、灵敏,适用于牛奶中光引发剂多残留的定量测定和确证。
建立瞭牛奶中11種光引髮劑殘留的定性和定量測定分析方法。樣品經Carrez試劑沉澱蛋白質後,使用乙腈提取,HLB固相萃取柱淨化,乙腈洗脫,洗脫液用氮氣吹榦後用50%乙腈水溶液定容,採用液相色譜-串聯質譜進行測定。分析物採用電噴霧電離,正離子掃描,多反應鑑測(MRM)模式檢測,其中7種光引髮劑使用內標法定量,4種光引髮劑使用外標法定量。11種光引髮劑在5.00~200μg/L濃度範圍內線性關繫良好,相關繫數均大于0.990。11種光引髮劑的測定低限均為1.0μg/kg。在添加濃度1.00~100μg/kg範圍內,加標迴收率為74.3%~112%,相對標準偏差為0.57%~16.3%。本方法簡便、有效、靈敏,適用于牛奶中光引髮劑多殘留的定量測定和確證。
건립료우내중11충광인발제잔류적정성화정량측정분석방법。양품경Carrez시제침정단백질후,사용을정제취,HLB고상췌취주정화,을정세탈,세탈액용담기취간후용50%을정수용액정용,채용액상색보-천련질보진행측정。분석물채용전분무전리,정리자소묘,다반응감측(MRM)모식검측,기중7충광인발제사용내표법정량,4충광인발제사용외표법정량。11충광인발제재5.00~200μg/L농도범위내선성관계량호,상관계수균대우0.990。11충광인발제적측정저한균위1.0μg/kg。재첨가농도1.00~100μg/kg범위내,가표회수솔위74.3%~112%,상대표준편차위0.57%~16.3%。본방법간편、유효、령민,괄용우우내중광인발제다잔류적정량측정화학증。
A method for the qualitative and quantitative determination of 11 photoinitiators residues in milk by liquid chroma-tography-tandem mass spectrometry (LC-TMS) was developed.The samples were extracted with acetonitrile after being precipi-tated by Carrez reagent, and then cleaned by HLB solid phase extraction cartridge .The analytes were eluted by acetonitrile , and then reconstituted by 50%acetonitrile aqueous solution after being dried by nitrogen gas .LC-TMS was used for the determination. The analytes were determined by the mode of electro -spray ionization (ESI), positive ion scan, and multiple reaction monitoring (MRM), and internal standard method for the quantification of 7 photoinitiators and external standard method for the quantification of other 4 photoinitiators were used.Eleven photoinitiators within the concentration range of 5.00~200μg/L showed good linear re-lationship with the correlation coefficient of more than 0.990.All the lowest limits of the quantitative determination were 1.00 μg/kg.The recoveries of 11 photoinitiators were between 74.3%and 112% when the adding concentrations were 1.00~100 μg/kg, and the relative standard deviations varied from 0.57%to 16.3%.This method was simple, effective and sensitive, and suitable for the quantitative determination and confirmation of photoinitiator residues in milk .