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HPLC及LC-MS测定榛子中氯吡苯脲和多菌灵残留

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本文采用高效液相色谱法(HPLC)和液相色谱-质谱法(LC-MS)对干果榛子中氯吡苯脲和多菌灵残留量进行含量测定.HPLC 和 LC-MS 均使用 C18 色谱柱,含量测定采取等度洗脱,流动相:甲醇-水(55∶45,体积比);体积流量:1.0 mL·min-1;测定波长:260 nm;柱温:30℃.LC-MS采取电喷雾离子源,梯度洗脱,体积流量:0.6 mL·min-1,柱温:30℃.结果表明,榛子中氯吡苯脲与多菌灵存在残留,氯吡苯脲质量浓度在1.00~10.00 μg·mL-1范围内线性关系良好,加样回收率在 95.58%~100.58%;多菌灵质量浓度在1.005~15.075 μg·mL-1范围内具有良好的线性关系,加样回收率在 95.61%~104.39%.实验证明,HPLC与LC-MS相结合的方法具有操作简便、灵敏度高、检出限低等优点,能有效地检测到榛子样品中膨大剂氯吡苯脲及杀菌剂多菌灵的残留,并确定其残留量,线性关系和回收率结果均令人满意.根据被检测的8 批样品中氯吡苯脲和多菌灵两项农药残留量推断,作为一般干果食用榛子是安全的.
Determination of Chlorfenuron and Carbendazim in Hazelnut by HPLC and LC-MS
In this study,high performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC-MS)are used to determine the residual content of chlorfenuron and carbendazim in dried hazelnuts.Both HPLC and LC-MS use C18 chromatographic columns,and the content determination adopts isocratic elution.Mobile phase:methanol-water(55∶45 by volume);volume flow:1.0 mL·min-1;measurement wavelength:260 nm;column temperature:30℃.LC-MS uses electrospray ion source,gradient elution,volume flow rate:0.6 mL·min-1,column temperature:30℃.The results show that there are residues of chlorfenuron and carbendazim in hazelnuts.The content of chlorfenuron hand good linearity in the range of 1.00~10.00 μg·mL-1.The sample recovery rate is 95.58%~100.58%;the content of carbendazim is 1.005~15.075 μg·mL-1,and the sample recovery rate is 95.61%~104.39%.Experiments have proved that the establishment of the method combining HPLC with LC-MS has the advantages of simple operation,high sensitivity and low detection limit,and can effectively detect the bulking agent chlorfenuron and more fungicides in hazelnut samples.The residues of bacteriostat were determined,and the results of linearity and recovery were satisfactory.According to the two pesticide residues of chlorfenuron and carbendazim in the 8 batches of samples tested,it is inferred that hazelnuts are safe to eat as general dried fruits.

hazelnutchlorfenuroncarbendazimhigh performance liquid chromatography(HPLC)liquid chromatography-mass spectrometry(LC-MS)

桑育黎、王沛、郝延军、李楠楠、戚建忠

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辽宁大学 药学院,辽宁 沈阳 110036

辽宁中医药大学 中医药科学院,辽宁 沈阳 110847

华润三九(郴州)制药有限公司,湖南 郴州 423000

榛子 氯吡苯脲 多菌灵 高效液相色谱法(HPLC) 液相色谱-质谱法(LC-MS)

辽宁大学大学生创新创业训练计划辽宁大学大学生创新创业训练计划

D201911231532324418D2019911231644210910

2024

辽宁大学学报(自然科学版)
辽宁大学

辽宁大学学报(自然科学版)

影响因子:0.371
ISSN:1000-5846
年,卷(期):2024.51(1)
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