固相萃取超高效液相色谱串联质谱法同时测定贝类产品中脂溶性贝类毒素
PDF下载 (11392)柴继业1,王琳1,赵巧灵2,黄朱梁2,史西志1*,孙爱丽1,李德祥1.固相萃取超高效液相色谱串联质谱法同时测定贝类产品中脂溶性贝类毒素[J].宁波大学学报(理工版),2018,31(3):65-71.DOI:
CHAI Ji-ye1,WANG Lin1,ZHAO Qiao-ling2,HUANG Zhu-liang2,SHI Xi-zhi1*,SUN Ai-li1,LI De-xiang1.A solid phase extraction-ultrahigh performance liquid chromatography-tandem mass spectrometry method for the determination of lipophilic marine toxins in shellfish[J].Journal of Ningbo University(Natural Science & Engineering Edition),2018,31(3):65-71.DOI:
| Title: | A solid phase extraction-ultrahigh performance liquid chromatography-tandem mass spectrometry method for the determination of lipophilic marine toxins in shellfish |
| 作者: | 柴继业1, 王琳1, 赵巧灵2, 黄朱梁2, 史西志1*, 孙爱丽1, 李德祥1 |
| Author(s): | CHAI Ji-ye1, WANG Lin1, ZHAO Qiao-ling2, HUANG Zhu-liang2, SHI Xi-zhi1*, SUN Ai-li1, LI De-xiang1 |
| 关键词: | 脂溶性贝类毒素; 超高效液相色谱-串联质谱法; 石墨烯; 固相萃取 |
| Keywords: | lipophilic marine toxins; ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); oxide-graphene; solid phase extraction |
| 分类号: | O657.63 |
| 文献标识码: | A |
| 摘要: | 建立基于氧化石墨烯的Spin-mini固相萃取小柱样品净化超高效液相色谱串联质谱同时测定贝类产品中脂溶性贝类毒素的方法. 样品采用V甲醇V(乙醇V(异丙醇7:2:1振荡提取, 经氧化石墨烯Spin-mini固相萃取小柱净化, 并利用超高效液相色谱串联质谱法进行检测, 外标法定量. 大环内酯类贝类毒素-2(PTX2)、米氏裸甲藻毒素(Gymnodimine, GYM)线性范围为3.030.0μg·kg-1, 原多甲藻酸(Azaspiracids, AZA1、AZA2、AZA3)线性范围为0.7510.0μg·kg-1, 螺环内酯毒素(13-Desmethyl pirolide C, SPX1)线性范围为3.040.0μg·kg-1, 相关系数均大于0.99, 方法检限范围为0.100.26μg·kg-1, 定量限范围为0.280.81μg·kg-1. 在贝类样品基质中6种脂溶性贝类毒素3个添加水平的平均回收率为82.5115.7％, 相对标准偏差为0.914.3％. 该方法具有操作时间短、有机溶剂用量少、灵敏度高、回收率和稳定性较好等优势, 适用于贝类样品中多种脂溶性贝类毒素残留的检测与确证. |
| Abstract: | A spin-mini solid phase extraction (SPE) based on the oxide graphene coupled with ultra performance liquid chromatography-electrospray ionization trap tandem mass spectrometry (UPLC-MS/MS) was developed to determine six lipophilic marine toxins (LPTs) in shellfish. Samples were firstly extracted with methanol: ethanol:isopropanol (7:2:1), purified with spin-mini solid phase extraction based on oxide grapheme. The analytes were analyzed by UPLC-MS/MS by an external standard method. The calibration curves of PTX2 and GYM showed good linearity in the range of 3.0?30.0μg·kg-1. AZA1, AZA2, AZA3 showed good linearity in the range of 0.75?10.0μg·kg-1. SPX1 showed good linearity in the range of 3.0?40.0μg·kg-1, with linear correlation coefficient above 0.9932. The limits of detection (LODs) and limits of quantification (LOQs) were 0.10?0.26μg·kg-1 and 0.28?0.81μg·kg-1 respectively. The average recovery of 3 levels of 6 LPTs in shellfish samples was 82.5%?115.7%, and the relative standard deviation was 0.9%?14.3%. The proposed method is efficient with low solvent consumption, high sensitivity, improved recovery and stability. The method can be used for the determination and verification of LPTs in shellfish. |
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| 备注/Memo: | 收稿日期: 2017?11?17. 宁波大学学报（理工版）网址: http://journallg.nbu.edu.cn/ 基金项目: 国家自然科学基金（31372572）; 海洋公益性行业科研专项（201305010）; 浙江省食品药品监管系统科技计划项目（2015002）; 宁波市科技创新团队项目（2015C110018）; 宁波大学学科项目（XKZSC1515, XKZSC1412）. 第一作者: 柴继业（1992－）, 男, 安徽阜阳人, 在读硕士研究生, 主要研究方向: 食品安全. E-mail: chaijiye@163.com *通信作者: 史西志（1979－）, 男, 山东淄博人, 博士/教授, 主要研究方向: 水产品安全. E-mail: shixizhi@nbu.edu.cn 宁波大学学报（理工版）网址：http://journallg.nbu.edu.cn/ |
