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[url=https://insevent.instrument.com.cn/t/Mp]气相[/url]要用顶空测青霉素钾盐中的正丁醇、乙酸乙酯的残留,可样品不溶于DMS和DMSO溶剂,能溶于水,但正丁醇和乙酸乙酯不溶于水,能进样检测吗?
LC-MS/MS 测定牛奶中六种青霉素类抗生素残留黄百芬 莫燕霞 任一平浙江省疾病预防控制中心 中国浙江省杭州 310009 本文建立了应用LC-MS/MS 快速测定牛奶中六种青霉素类抗生素残留的方法。采用液相色谱-电喷雾串联四极杆质谱仪,多离子反应监测(MRM)定量。通过对试样净化预处理、色谱条件、质谱参数等的优化选择和方法回收率、精密度等的验证,建立了定量测定牛奶中青霉素类抗生素含量的理想方法。实验结果表明,方法检出限:青霉素G0.02ng/mL、青霉素V 0.06ng/mL、苯唑西林 0.04ng/mL、氯唑西林 0.11ng/mL、奈夫西林0.02ng/mL、双氯唑西林0.19ng/mL;在0.2-2.0ng/mL 浓度范围内,相关系数R 为0.991,回收率大于90%,方法精密度RSD 为4.87%。结论采用液相色谱-电喷雾串联四极杆质谱仪,可快速测定牛奶中六种以上青霉素类抗生素残留的含量,结果准确可靠,重复性好,灵敏度高。 液相色谱-电喷雾串联质谱、牛奶、青霉素类、残留Determination of β-Lactam Residues in Milk by Liquid ChromatographyTandem Mass SpectrometryHuang Baifen Mo Yanxia Ren YipingZhejiang Provincial Center for Disease Prevention and Control,Hangzhou 310009Abstract Liquid chromatography coupled with electrospray ionization tandem massspectrometry (LC-MS/MS) was applied to the quantification of β-lactam residues in milk. Thesamples was cleaned up and concentrated by solid phase extraction (SPE) with OASIS HLBcartridges. β-lactams were detected with a C18 column using acetonitriLe (0.1% acid) andwater(0.1% acid) as mobile phase. The Linear range was from 0.2ng/mL to 20.0ng/mL, r=0.991.The average recovery is above 90%, RSD=4.87%(n=6). The analytical method in the presentstudy was well validated and good results were obtained with respect to precision, repeatabilityand spiked recovery.Keywords HPLC-MS/MS;β-lactam residues, milk
青霉素一般比较不稳定,好多奶农在牛奶加酶去分解,大家有什么好的办法来测定牛奶中青霉素的含量?我们这里有LCMSMS,GC LC ,定量的话用LC-MSMS但是不稳定?