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加工处理对鲢小清蛋白免疫活性的影响
  • ISSN号:1000-0615
  • 期刊名称:水产学报
  • 时间:2013.2.2
  • 页码:297-302
  • 分类:O657.63[理学—分析化学;理学—化学]
  • 作者机构:[1]集美大学食品与生物工程学院,福建厦门361021, [2]厦门市农产品质量安全检验测试中心,福建厦门361009
  • 相关基金:国家自然科学基金(31171660)
  • 相关项目:基质金属蛋白酶对鱼类肌肉胶原蛋白的作用机理研究
中文摘要:

利用QuEChERS前处理结合高效液相色谱-串联质谱(HPLC-MS/MS),建立同时检测红薯中11种地下杀虫剂的痕量残留分析方法.通过优化确定了乙腈提取、乙二胺-N-丙基硅烷(PSA)为净化剂的QuEChERS前处理方法;采用水(含0.1%甲酸,5%乙腈)和乙腈(含0.1%甲酸,5%水)梯度洗脱,Venusil MP C18色谱柱分离,电喷雾电离正离子(ESI+)模式、多反应监测方式(MRM)测定,以及空白基质外标法定量.结果显示,11种地下杀虫剂的保留时间≤10min,在各自的范围内线性关系良好,R2〉0.999 0;方法的检出限(LOD)为0.007-4.000μg/kg,定量限(LOQ)为0.023-13.333μg/kg;空白红薯分别添加5,10,20和50μg/kg 4个含量水平,11种地下杀虫剂的平均回收率为81.7%-117.2%,相对标准偏差(RSD)为1.4%-8.3%.结果表明,本研究建立的QuEChERS-HPLC-MS/MS方法简单、快速,灵敏度、准确度符合要求,适用于红薯中多种地下杀虫剂痕量残留的同时检测.

英文摘要:

In this study a method has been developed for simultaneous and multiresidue analysis of 11 types of trace level under- ground pesticides in sweet potatoes by QuEChERS and high-performance liquid chromatography tandem mass spectrometry(HPLC- MS/MS). Sample pretreatment conditions and HPLC-MS/MS conditions were optimized. From sweet potatoes acetonitrile was directly extracted,and pesticides were purified using primary secondary amine (PSA) with QuEChERS method. 0.1% HAc Acetonitrile-water (5:95,by volume) and 0.1% H Ac acetonitrile-water (95:5, by volume) were chose to be mobile with gradient elution, and then they were analyzed using HPLC-MS/MS in multiple reaction monitoring (MRM) modes via positive electrospray ionization (ESI+ ) with an Venusil MP C18 column (3 μm,2.1 mm×100 mm) as the analytical column,and the quantization was carried out by the external standard method with the blank matrix. The chromatographic peaks of 11 types of underground pesticides were flowed out within 10 minutes. Data demonstrated that the linear correlation coefficients for 11 types of pesticides were not less than 0. 999 0 in their linear scope with good linearity. The limit of detection (LOD) ranged from 0. 007 to 4. 000 μg/kg,and the limit of quantization (LOQ) was in the range of 0. 023 to 13. 333 μg/kg. The recoveries of 11 types of underground pesticides in sweet potato matri- ces at four spiked levels of 5,10,20,and 50 μg/kg ranged from 81.7 % to 117.2%, and the relative standard deviations were in the range of 1.4% to 8.3 %. The results showed that the method is simple,rapid, and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.

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期刊信息
  • 《水产学报》
  • 中国科技核心期刊
  • 主管单位:中国科协
  • 主办单位:中国水产学会
  • 主编:黄硕琳
  • 地址:上海市军工路334号上海水产大学
  • 邮编:201306
  • 邮箱:jfc@shou.edu.cn
  • 电话:021-61900228
  • 国际标准刊号:ISSN:1000-0615
  • 国内统一刊号:ISSN:31-1283/S
  • 邮发代号:4-297
  • 获奖情况:
  • 曾先后三次获中国科协专项基金资助,获首届《CAJ-CD规范》执行优秀奖,获水产类期刊一等奖
  • 国内外数据库收录:
  • 美国化学文摘(网络版),英国农业与生物科学研究中心文摘,美国剑桥科学文摘,英国动物学记录,日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),中国北大核心期刊(2000版)
  • 被引量:26128