同位素内标法—超高效液相色谱/串联质谱法测定六堡茶中苦参碱和氧化苦参碱残留量
CSTR:
作者:
作者单位:

(1. 梧州学院食品与制药工程学院,广西 梧州 543002;2. 梧州学院六堡茶现代产业学院,广西 梧州 543002;3. 梧州学院体育健康学院,广西 梧州 543002;4. 梅河口市食品药品检验检测中心,吉林 梅河口 135000)

作者简介:

石金娥,女,梧州学院正高级工程师,博士。

通讯作者:

奚广生(1967—),男,梧州学院教授,博士。E-mail: 1790341091@qq.com

中图分类号:

基金项目:

广西科技重大专项(编号:桂科AA22068085)


Determination the residues of matrine and oxymatrine in Liupao tea by UPLC-MS/MS with isotope internal standard method
Author:
Affiliation:

(1. School of Food and Pharmaceutical Engineering, Wuzhou College, Wuzhou, Guangxi 543002, China;2. Liupao Tea Modern Industry College, Wuzhou College, Wuzhou, Guangxi 543002, China;3. School of Physical Education and Health, Wuzhou College, Wuzhou, Guangxi 543002, China;4. Meihekou Center for Food and Drug Control, Meihekou, Jilin 135000, China)

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    摘要:

    目的:以广西六堡茶为例,建立超高效液相色谱—质谱/质谱(UPLC-MS/MS)分析方法测定苦参碱和氧化苦参碱残留量。方法:样品经乙腈水溶液(80%乙腈+0.2%氨水)超声提取,流动相为0.1%甲酸—水和0.1%甲酸—甲醇溶液,梯度洗脱,内标法定量。结果:苦参碱和氧化苦参碱在0.1~80.0 ng/mL质量浓度范围内呈线性,相关系数均>0.999 6,检出限均为1.0 μg/kg,定量限均为3.0 μg/kg,满足茶叶中苦参碱和氧化苦参碱残留量的监管判定要求。通过加标验证,回收率均为92.0%~104.7%,相对标准偏差(RSD)均<5.4%。结论:试验方法结合净化管净化(147.7 mg PSA,15.1 mg GCB,887.2 mg硫酸镁),以Kinetex 2.6 μm Biphenyl 100 色谱柱(100 mm×3.0 mm)分离,解决了苦参碱和氧化苦参碱提取回收率低、前处理复杂的问题,使苦参碱和氧化苦参碱出峰良好,抗干扰性强。

    Abstract:

    Objective: Taking Guangxi Liupao tea as an example, an UPLC-MS/MS analysis method with residual amounts of matrine and Oxymatrine was established. Methods: The prepared samples were subjected to optimized acetonitrile aqueous solution (80% acetonitrile+0.2% ammonia water) ultrasonic extraction, mobile phase: formic acid water and formic acid methanol (both 0.1%), gradient elution, and internal standard method quantification. Results: It was linear in the range of 0.1~80.0 ng/mL, r was greater than 0.999 6, the detection limits of matrine and oxymatrine were 1.0 μg/kg, and the quantitative limits were 3.0 μg/kg, which met the regulatory determination requirements for the residue of matrine and oxidative matrine in tea. Through the spike verification, the recovery rate was in the range of 92.0%~104.7%, and the relative standard deviation (RSD) was less than 5.4%. Conclusion: Method combined with purification tube purification (147.7 mg PSA, 15.1 mg GCB, 887.2 mg magnesium sulfate), using Kinetex 2.6 μm Biphenyl 100  chromatographic column (100 mm×3.0 mm) separation solves the problems of low extraction recovery rate and complex pre-treatment of matrine and oxymatrine, so that the symmetrical peak shape and strong anti-interference ability of matrine and oxymatrine.

    参考文献
    相似文献
    引证文献
引用本文

石金娥,张洪禹,辛若竹,等.同位素内标法—超高效液相色谱/串联质谱法测定六堡茶中苦参碱和氧化苦参碱残留量[J].食品与机械,2024,40(3):89-94.
SHI Jine, ZHANG Hongyu, XIN Ruozhu, et al. Determination the residues of matrine and oxymatrine in Liupao tea by UPLC-MS/MS with isotope internal standard method[J]. Food & Machinery,2024,40(3):89-94.

复制
分享
文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2023-07-18
  • 最后修改日期:
  • 录用日期:
  • 在线发布日期: 2024-04-30
  • 出版日期:
文章二维码
×
《食品与机械》
友情提示
友情提示 一、 近日有不少作者反应我刊官网无法打开,是因为我刊网站正在升级,旧网站仍在百度搜索排名前列。请认准《食品与机械》唯一官方网址:http://www.ifoodmm.com/spyjx/home 唯一官方邮箱:foodmm@ifoodmm.com; 联系电话:0731-85258200,希望广大读者和作者仔细甄别。