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中国精品科技期刊2020
曾广丰, 刘青, 王志元, 丁博, 陈文锐, 韦晓群, 李文斌, 胡志玲, 韩深. QuEChERS法结合高效液相色谱-高分辨飞行时间质谱测定食用贝类产品中4种脂溶性贝类毒素[J]. 食品工业科技, 2015, (21): 289-294. DOI: 10.13386/j.issn1002-0306.2015.21.051
引用本文: 曾广丰, 刘青, 王志元, 丁博, 陈文锐, 韦晓群, 李文斌, 胡志玲, 韩深. QuEChERS法结合高效液相色谱-高分辨飞行时间质谱测定食用贝类产品中4种脂溶性贝类毒素[J]. 食品工业科技, 2015, (21): 289-294. DOI: 10.13386/j.issn1002-0306.2015.21.051
ZENG Guang-feng, LIU Qing, WANG Zhi-yuan, DING Bo, CHEN Wen-rui, WEI Xiao-qun, LI Wen-bin, HU Zhi-ling, HAN Shen. Determination of four lipophilic shellfish toxins in edible shellfishes by Qu ECh ERS technology combined with high performance liquid chromatography- high resolution time of flight mass spectrometry[J]. Science and Technology of Food Industry, 2015, (21): 289-294. DOI: 10.13386/j.issn1002-0306.2015.21.051
Citation: ZENG Guang-feng, LIU Qing, WANG Zhi-yuan, DING Bo, CHEN Wen-rui, WEI Xiao-qun, LI Wen-bin, HU Zhi-ling, HAN Shen. Determination of four lipophilic shellfish toxins in edible shellfishes by Qu ECh ERS technology combined with high performance liquid chromatography- high resolution time of flight mass spectrometry[J]. Science and Technology of Food Industry, 2015, (21): 289-294. DOI: 10.13386/j.issn1002-0306.2015.21.051

QuEChERS法结合高效液相色谱-高分辨飞行时间质谱测定食用贝类产品中4种脂溶性贝类毒素

Determination of four lipophilic shellfish toxins in edible shellfishes by Qu ECh ERS technology combined with high performance liquid chromatography- high resolution time of flight mass spectrometry

  • 摘要: 建立了Qu ECh ERS净化技术结合高效液相色谱-高分辨飞行时间质谱法测定食用贝类产品中4种脂溶性贝类毒素(Okadaic Acid,OA、Spirolides1,SPX1、Dinophysistoxin1,DTX1、Azaspiracid1,AZA1)的快速方法。以Qu ECh ERS净化技术对食用贝类样品进行提取与净化后,经C18色谱柱分离,用高分辨飞行时间质谱仪(ESI源)进行测定。用Peak View软件对分析结果进行全智能分析,对照每个样品与标准品的TOF-MS质量精度及同位素分布情况、保留时间以及TOF-MS/MS谱图,对化合物作出定性判断。同时利用Multi Quant软件对四种毒素进行外标法定量,OA和DTX1的线性范围为2.0100μg/L,方法检出限为10μg/kg;AZA1和SPX1的线性范围为0.520μg/L,方法检出限为2.0μg/kg,相关系数(R2)均大于0.997。高、中、低三个添加水平的平均回收率在75.6%94.1%之间,RSD小于10%。应用该方法对进出口的贻贝、北极贝、象拔蚌、牡蛎等20个样品进行检测,发现8个样品的SPX1和2个AZA1测定结果为阳性。该方法操作简便、高效快速、灵敏度高、重现性好,适用于贝类产品中脂溶性贝类毒素的检测。 

     

    Abstract: A determination method of four lipophilic shellfish toxins ( Okadaic Acid, OA; Spirolides1, SPX1;Dinophysistoxin1, DTX1; Azaspiracid1, AZA1) in edible shellfish products by Qu ECh ERS technology combined with high performance liquid chromatography- high resolution time of flight mass spectrometry ( HPLC- TOF- MS / MS) was established.Qu ECh ERS technology was used to extract and purify the samples.Four lipophilic shellfish toxins were separated by C18 column and detected by HPLC- TOF- MS / MS at electrospray ionization ( ESI) mode. After importing data by Peak View software, TOF-MS/ MS quality precision, isotopic distribution and retention time of each compounds, as well as the MS2 chromatogram of the standard solution and sample were compared to qualitatively analyze the target compound.Finally, the software of Multi Quant was used to quantify by external standard calibration method.The calibration curves of OA and DTX1 showed good linearity in the range of 2.0 ~ 100 μg / L, the limits of detection ( LOD, S / N = 3) were 10 μg / kg, while the LOD of AZA1 and SPX1 were 2.0 μg / kg, the ranges werebetween 0.520 μg / L.The correlation coefficients ( R2) were all above 0.997.The average spiked recoveries of four shellfish toxins at three concentration levels were between 75.6% ~ 94.1%, and RSD all below 10%. 20 import &export samples including mussel, octopus, geoduck and oyster were screened by the developed method, SPX1 was found in 8 samples and AZA1 in 2 samples. The developed method was easy, quick, sensitive, reproducible and suitable for the determination of lipophilic shellfish toxins in shellfish products.

     

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