用实时直接分析质谱法(DART-MS)快速测定桑叶中的γ-氨基丁酸含量  

Rapid Determination of γ-Aminobutyric Acid Content in Mulberry Leaves Using Direct Analysis in Real Time Mass Spectrometry( DART-MS)

作　　者：李无双 郎文成 马琳 李龙 武国华 Li Wushuang;Lang Wencheng;Ma Lin;Li Long;Wu Guohua(College of Environmental and Chemical Engineering,Jiangsu University of Science and Technology,Zhenjiang Jiangsu 212018,China;Sericultural Research Institute,Chinese Academy of Agricultural Sciences,College of Biotechnology,Jiangsu University of Science and Technology,Zhenjiang Jiangsu 212018,China)

机构地区：[1]江苏科技大学环境与化学工程学院,江苏镇江212018 [2]中国农业科学院蚕业研究所、江苏科技大学生物技术学院,江苏镇江212018

出　　处：《蚕业科学》2018年第4期567-572,共6页ACTA SERICOLOGICA SINICA

基　　金：江苏省特聘教授专项基金项目(No.苏教师[2015]17);现代农业产业技术体系建设专项(No.CARS-18)

摘　　要：γ-氨基丁酸（γ-aminobutyric acid,GABA）是桑叶中具有多种药理作用的重要组分之一。为了快速、准确测定桑叶中的GABA含量,建立了基于实时直接分析电离源-串联三重四极杆质谱（DART-MS）的桑叶GABA定性和定量分析方法。在DART离子源和质量分析器同为正离子的模式下,采用选择反应监测模式（SRM）并选取m/z 104→87为定量离子对,以其峰面积（y）进行定量分析,所得线性回归方程为y=4 552 210.19x-11 927 811.70,线性系数R-2=0.998,且在GABA溶液质量浓度（x）为2.50-40.00μg/m L范围内的线性关系良好。对3种质量浓度（7.82、4.14、2.78μg/m L）桑叶样品提取液进行测定的相对标准偏差（RSD）分别为3.98%、5.60%、2.28%,表明该方法的精密度良好;加标回收率在85.60%-97.47%之间。应用DART-MS法对来源于江、浙、皖蚕区的6个桑品种的桑叶样品进行检测,桑叶提取液样品中的GABA质量浓度从高到低的桑品种依次为湖桑32号（7.82μg/m L±0.31μg/m L,江苏海安）、强桑2号（7.44μg/m L±0.21μg/m L,浙江杭州）、强桑1号（7.14μg/m L±0.50μg/m L,杭州）、农桑14号（5.88μg/m L±0.30μg/m L,杭州）、育711号（5.81μg/m L±0.18μg/m L,安徽合肥）、农桑14号（4.25μg/m L±0.29μg/m L,浙江海宁）。建立的DART-MS法用于测定桑叶中的GABA含量,具有简单、快速且灵敏度高等特点。γ-Aminobutyric acid（ GABA） is one of the important components with multiple physiological functions in mulberry leaves. In order to rapidly and accurately determine GABA content in mulberry leaves,a qualitative and quantitative analysis method for mulberry leaf GABA based on direct analysis in real time ionization source and tandem triple quadrupole mass spectrometry（ DART-MS） was established. Both DART ion source and mass analyzer were set in the positive ion mode. The selective reaction monitoring mode（ SRM）was used,m/z 104→87 was selected as the quantitative ion pair,and the peak area（ y） was used for quantitative analysis. The obtained linear regression equation was y =4 552 210. 19 x-11 927 811. 70,the linear coefficient R-2=0. 998,and the linear relationship was good while the mass concentration range（ x） of GABA solution was at2. 50-40. 00 μg/m L. The relative standard deviations（ RSDs） of the three mulberry leaf extractions（ 7. 82,4. 14 and 2. 78 μg/m L） were 3. 98%,5. 60% and 2. 28%,respectively,indicating that the precision of the method was good. The range of spiked recovery was shown to be 85. 60%-97. 47%. The mulberry leaf samples from six mulberry varieties collected in Jiangsu,Zhejiang,and Anhui sericulture areas were detected by this method. The GABA contents in mulberry leaf extractions were in the order of（ from high to low） ： Husang 32（ 7. 82 μg/m L±0. 31 μg/m L,Hai＇an,Jiangsu）,Qiangsang 2（ 7. 44 μg/m L±0. 21 μg/m L,Hangzhou,Zhejiang）,Qiangsang 1（ 7. 14 μg/m L±0. 50 μg/m L,Hangzhou）,Nongsang 14（ 5. 88 μg/m L±0. 30 μg/m L,Hangzhou）,Yu 711（ 5. 81 μg/m L±0. 18 μg/m L,Hefei,Anhui）,and Nongsang 14（ 4. 25 μg/m L±0. 29 μg/m L,Haining,Zhejiang）. The DART-MS method developed in this study is simple,rapid,and highly sensitive for determination of GABA in mulberry leaves.

关 键 词：实时直接分析质谱 桑叶 Γ-氨基丁酸 精密度 加标回收率 

分 类 号：O657.63[理学—分析化学] R284.3[理学—化学]