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中国精品科技期刊2020
吴婉琴,江丰,范小龙,等. 高效液相色谱-串联质谱法测定畜禽肉及其制品中工业松香[J]. 食品工业科技,2021,42(12):279−286. doi: 10.13386/j.issn1002-0306.2020080257.
引用本文: 吴婉琴,江丰,范小龙,等. 高效液相色谱-串联质谱法测定畜禽肉及其制品中工业松香[J]. 食品工业科技,2021,42(12):279−286. doi: 10.13386/j.issn1002-0306.2020080257.
WU Wanqin, JIANG Feng, FAN Xiaolong, et al. Determination of Rosin in Meat and Their Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(12): 279−286. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020080257.
Citation: WU Wanqin, JIANG Feng, FAN Xiaolong, et al. Determination of Rosin in Meat and Their Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(12): 279−286. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020080257.

高效液相色谱-串联质谱法测定畜禽肉及其制品中工业松香

Determination of Rosin in Meat and Their Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 为建立高效液相色谱-串联质谱(HPLC-MS/MS)检测畜禽肉及其制品中工业松香的分析方法。样品经乙腈溶液超声提取,经C18固相萃取柱净化,定容过滤膜后采用HPLC-MS/MS对目标物脱氢松香酸进行分析,内标法定量。采用Waters ACQUITY HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm)分离,以0.1%甲酸(v/v)水溶液和乙腈(30:70)为流动相进行等度洗脱,采用电喷雾电离(ESI)源、多反应监测(MRM)、正离子扫描模式进行检测。结果表明,在5~400 ng/mL的范围内目标化合物呈现较好的线性关系(相关系数r>0.99),检出限(LOD)和定量限(LOQ)分别为80和200 μg/kg。目标化合物在200、400和2000 μg/kg 3个水平下的加标平均回收率为96.05%~104.17%,相对标准偏差(RSD)为0.62%~3.68%(n=6)。实际样品检测分析结果显示,脱氢松香酸阳性样品数量占样品总量的16.67%,残留含量范围为390.15~1850.03 μg/kg。该法简便快捷,准确可靠,可适用于畜禽肉及其制品中工业松香的快速准确测定。

     

    Abstract: To establish a method for the determination of rosin in meat and their products by using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), the sample was extracted by ultrasonic instrument with acetonitrile. The extracts were then purified through solid-phase extraction (SPE) with C18 cartridges. The target of dehydroabietic acid was analyzed by HPLC-MS/MS, and quantified by internal standard method. The separation was performed on a Waters ACQUITY HSS T3 column (2.1 mm×100 mm, 1.8 μm) with isometric elution using 0.1%(v/v)formic acid aqueous solution-acetonitrile (30:70) as the mobile phase.The analysis of dehydroabietic acid was detected under electrospray positive ionization mode and the multiple reaction monitoring(MRM) mode. The dehydroabietic acid demonstrated good linearity in the range of 5~400 ng/mL, with the correlation coefficient values (r) being higher than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) were found to be 80 and 200 μg/kg. The recoveries at three spiked levels (200, 400 and 2000 μg/kg) in blank matrix were in the range of 96.05%~104.17% with the relative standard deviations between 0.62%~3.68% (n=6). The analysis results of actual samples showed that the number of positive samples of dehydroabietic acid accounted for 16.67% of the total samples, and the residual content was in the range of 390.15~1850.03 μg/kg. The method was convenient, rapid, accurate and efficient. It could be employed for accurate determination of rosin in meat and their products.

     

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