色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
6期
652-656
,共5页
郑香平%丁立平%陈志涛%郭菁%张睿%吴文凡
鄭香平%丁立平%陳誌濤%郭菁%張睿%吳文凡
정향평%정립평%진지도%곽정%장예%오문범
超高效液相色谱%串联质谱法%噻菌灵%多菌灵%浓缩果汁
超高效液相色譜%串聯質譜法%噻菌靈%多菌靈%濃縮果汁
초고효액상색보%천련질보법%새균령%다균령%농축과즙
ultra-high performance liquid chromatography(UPLC)%tandem mass spectrome-try(MS/MS)%thiabendazole%carbendazim%concentrated fruit juices
建立了同时测定浓缩果汁中噻菌灵和多菌灵残留的超高效液相色谱-串联质谱快速检测法。样品用乙酸乙酯提取,以 ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)进行超高效液相色谱分离,以电喷雾电离串联质谱正离子多反应监测( MRM)模式进行测定,以基质匹配标准溶液外标法定量。结果表明:在试验条件下,噻菌灵和多菌灵在0.5~10μg/kg范围内线性关系良好,相关系数大于0.99,不同基质中的检出限( S/N=3)范围为0.12~0.23μg/kg。在0.5、1.0和5.0μg/kg 3个水平下噻菌灵和多菌灵的加标回收率为76.98%~108.7%,相对标准偏差( RSD)为2.95%~9.99%。同时,本研究对浓缩果汁中噻菌灵和多菌灵残留检测的基质效应进行了考察。本方法具有操作简便、快速、准确的特点,可用于浓缩果汁中噻菌灵和多菌灵残留量的日常检测。
建立瞭同時測定濃縮果汁中噻菌靈和多菌靈殘留的超高效液相色譜-串聯質譜快速檢測法。樣品用乙痠乙酯提取,以 ACQUITY UPLC BEH C18色譜柱(50 mm×2.1 mm,1.7μm)進行超高效液相色譜分離,以電噴霧電離串聯質譜正離子多反應鑑測( MRM)模式進行測定,以基質匹配標準溶液外標法定量。結果錶明:在試驗條件下,噻菌靈和多菌靈在0.5~10μg/kg範圍內線性關繫良好,相關繫數大于0.99,不同基質中的檢齣限( S/N=3)範圍為0.12~0.23μg/kg。在0.5、1.0和5.0μg/kg 3箇水平下噻菌靈和多菌靈的加標迴收率為76.98%~108.7%,相對標準偏差( RSD)為2.95%~9.99%。同時,本研究對濃縮果汁中噻菌靈和多菌靈殘留檢測的基質效應進行瞭攷察。本方法具有操作簡便、快速、準確的特點,可用于濃縮果汁中噻菌靈和多菌靈殘留量的日常檢測。
건립료동시측정농축과즙중새균령화다균령잔류적초고효액상색보-천련질보쾌속검측법。양품용을산을지제취,이 ACQUITY UPLC BEH C18색보주(50 mm×2.1 mm,1.7μm)진행초고효액상색보분리,이전분무전리천련질보정리자다반응감측( MRM)모식진행측정,이기질필배표준용액외표법정량。결과표명:재시험조건하,새균령화다균령재0.5~10μg/kg범위내선성관계량호,상관계수대우0.99,불동기질중적검출한( S/N=3)범위위0.12~0.23μg/kg。재0.5、1.0화5.0μg/kg 3개수평하새균령화다균령적가표회수솔위76.98%~108.7%,상대표준편차( RSD)위2.95%~9.99%。동시,본연구대농축과즙중새균령화다균령잔류검측적기질효응진행료고찰。본방법구유조작간편、쾌속、준학적특점,가용우농축과즙중새균령화다균령잔류량적일상검측。
A method was developed for the rapid determination of thiabendazole and carbenda-zim residues in concentrated fruit juices by using ultra-high performance liquid chromatography ( UHPLC)coupled with triple quadrupole tandem mass spectrometry( MS/MS),and quantified by matrix-matched standard solution in external standard method. The residues in the samples were extracted by ethyl acetate,and then analyzed by using UHPLC-MS/MS in multiple reac-tion monitoring( MRM)mode via positive electrospray ionization with an Waters ACQUITY UP-LC BEH C18 column(50 mm×2. 1 mm,1. 7 μm)as the analytical column. Good linearities were obtained in the range of 0. 5-10 μg/kg for both pesticides with correlation coefficients greater than 0. 99. The recovery experiments were carried out by spiking standards into blank samples of apple,peach,orange,pear,grape juices at three levels of 0. 5,1. 0 and 5. 0 μg/kg. The recoveries of thiabendazole and carbendazim were from 76. 98% to 108. 7% with the relative standard deviations( RSD)of 2. 95%-9. 99%. For both pesticides in different matrices,the lim-its of detection( S/N=3)were in the range of 0. 12-0. 23 μg/kg. Meanwhile,the pyrolysis mechanism and matrix effects for the determination of thiabendazole and carbendazim in con-centrated fruit juices were investigated in this study. The method is simple,rapid and accurate, and can be used for the routine analysis of thiabendazole and carbendazim in concentrated fruit juices.