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作 者:李洪权 柏玉冰 鲁翠香 赵东鲲 陈珉珉 陈晓燕 LI Hong-quan;BAI Yu-bing;LU Cui-xiang;ZHAO Dong-kun;CHEN Min-min;CHEN Xiao-yan(Department of Pharmacy,The Third Hospital of Changsha,Changsha 410035;Department of Pharmacy,The First Hospital of Hunan University of Chinese Medicine,Changsha 410007;Laboratory of Food Testing&Analysis,Zhuzhou Institute for Food and Drug Control,Zhuzhou Hunan 412000)
机构地区:[1]长沙市第三医院药学部,长沙410035 [2]湖南中医药大学第一附属医院药学部,长沙410007 [3]株洲市食品药品检验所食品分析检验研究室,湖南株洲412000
出 处:《中南药学》2022年第11期2621-2625,共5页Central South Pharmacy
基 金:湖南省市场监督管理局科技计划项目(No.2020KJJH42);《湖南省中药饮片炮制规范》(2010年版)修订。
摘 要:目的 建立起高效液相色谱-串联质谱法测定叶下珠中氯虫苯甲酰胺和氟虫双酰胺的残留量。方法 叶下珠粉末经乙腈超声提取,采用Welch Xtimate C18(4.6 mm×150 mm,5 μm)色谱柱,以乙腈-水为流动相等度洗脱,流速0.5 mL·min^(-1),柱温30℃,进样体积5 μL。采用电喷雾离子源进行正离子模式扫描。结果 氯虫苯甲酰胺和氟虫双酰胺均在1~100 ng·mL^(-1)与峰面积线性关系良好,检测限分别为0.3 μg·kg^(-1)和1.0 μg·kg^(-1),定量限分别为1.0 μg·kg^(-1)和3.0 μg·kg^(-1)。氯虫苯甲酰胺的含量范围为1.1~4.4 μg·kg^(-1),氟虫双酰胺未检出。结论 该方法高效、准确,可用于叶下珠中氯虫苯甲酰胺和氟虫双酰胺残留量的测定。Objective To determine chlorantraniliprole and flubendiamide residues in Phyllanthus urinaria L.by UPLC-MS/MS.Methods Phyllanthus urinaria L.powders were extracted by ultrasound with acetonitrile.Chromatographic separation was performed on a Welch Xtimate C18 column (4.6 mm×150 mm,5 μm).The mobile phase consisted of water (A) and acetonitrile (B) with isocratic elution.The flow rate was 0.5 mL·min^(-1).The column temperature was 30℃,and the injection volume was 5 μL.The mass spectrum was obtained by electrospray ionization under the positive ion mode.Results Chlorantraniliprole and flubendiamide showed good linearity at 1~100 ng·mL^(-1).The limit of detection was 0.3 μg·kg^(-1) and 1.0 μg·kg^(-1),respectively.The limit of quantitation was 1.0 μg·kg^(-1) and 3.0 μg·kg^(-1).The content of chlorantraniliprole was 1.1~4.4 μg·kg^(-1),while that of flubendiamide was not detected.Conclusion This method is highly efficient and accurate,which can be used for the determination of chlorantraniliprole and flubendiamide residues in Phyllanthus urinaria L..
关 键 词:叶下珠 氯虫苯甲酰胺 氟虫双酰胺 高效液相色谱-串联质谱法
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