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作 者:闫琪颖 王晓蕾 苏建 景永帅[1] 刘永利 刘玉真[1] YAN Qi-ying;WANG Xiao-lei;SU Jian;JING Yong-shuai;LIU Yong-li;LIU Yu-zhen(Hebei University of Science and Technology,Shijiazhuang 050018,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China)
机构地区:[1]河北科技大学,石家庄050018 [2]河北省药品医疗器械检验研究院,石家庄050227
出 处:《药物分析杂志》2023年第4期644-659,共16页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:建立北沙参中161个农药残留量的检测方法,了解全国流通领域药材与饮片的残留情况,统计识别产地差异。方法:采用QuEChERS前处理技术,气相色谱-串联质谱和液相色谱-串联质谱法同时测定北沙参中161个农药化合物残留量,运用统计分析技术分析主产地农药残留数据。结果:625批样品中400批检出24种农药及植物生长调节剂,检出率为64.00%,超标率为2.24%。各检出农药线性关系良好,3水平加标平均回收率均在70%~120%,RSD<20%。禁用农药滴滴涕的残留具有普遍性,毒死蜱、丙环唑、丙溴磷、氟乐灵、多效唑是产地差异的主导因子。结论:方法可应用于北沙参农残筛查,近2年我国北沙参农残检出率高,超标率低,剧毒高残留禁用农药土壤蓄积影响仍在,北沙参农药残留存在明显地域性差异。Objective:To establish a method for the determination of 161 pesticide residues in Radix Glehniae,to understand the residual situation of medicinal materials and decoction pieces in the national circulation field,and to identify the differences of habitats statistically.Methods:The QuEChERS(quick,easy,cheap,effective,rugged and safe)method was used for sample preparation,gas chromatography-tandem mass spectrometry and liquid chromatography-tandem mass spectrometry were used to simultaneously determine the residues of 161 pesticide compounds in Radix Glehniae,and the data of pesticide residues in samples from main habitats were analyzed by statistical analysis.Results:Among 625 batches of samples,24 kinds of pesticide and plant growth regulator residues were detected in 400 batches,the detection rate was 64.00%,and the over standard rate was 2.24%.The linear relationship among varieties was good.The average recoveries of three-level spiked standards were between 70%-120%with RSDs below 20%.The residues of banned pesticides DDT were common.Chlorpyrifos,propiconazole,profenofos,trifluralin and paclobutrazol were the dominant factors of differential expression of habitats.Conclusion:The method can be applied to the screening of pesticide residues in Radix Glehniae.In the past two years,the detection rate of agricultural residues of Radix Glehniae in China is high,the over standard rate is low,the highly toxic residue is high,and the influence of banned pesticide on soil accumulation is still.There are obvious regional differences in pesticide residues of Radix Glehniae.
关 键 词:北沙参 农残残留 多元统计分析 多效唑 氟乐灵 毒死蜱 滴滴涕 地域差异
分 类 号:R917[医药卫生—药物分析学]
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