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作 者:张楠楠 吕光达 王志强 黄艳梅 施志顺 ZHANG Nan-nan;LV Guang-da;WANG Zhi-qiang;HUANG Yan-mei;SHI Zhi-shun(Bozhou Products Quality Suoervision and Inspection Institute,Anhui Bozhou 236800;National Center for Quality Inspection and Testing of Traditional Chinese Medicinal Products(Anhui),Anhui Bozhou 236800;Bozhou Hanliangwuyou Chinese Medicine Testing Co.,Ltd.,Anhui Bozhou 236800,China)
机构地区:[1]亳州市产品质量监督检验所,安徽亳州236800 [2]国家中药材产品质量检验检测中心,安徽亳州236800 [3]亳州含量无忧中药材检测有限公司,安徽亳州236800
出 处:《广州化工》2024年第4期110-114,共5页GuangZhou Chemical Industry
摘 要:建立气相色谱串联质谱仪与超高效液相色谱串联质谱仪测定方法,通过内标法与外标法共同定量分析。用乙腈提取并用平行真空浓缩仪低温浓缩乙腈,再用乙腈稀释溶解样品最后通过亲水亲油平衡材料固相萃取柱净化,评价二年生白术中药材受33种禁用农药的污染情况,结果表明,33种禁用农药标准曲线线性良好,相关系数均大于0.99,准确性与重复性回收率在61%~118%之间。30批二年生白术、甲拌磷、氟虫腈、甲基异柳磷检出,检出率为66.6%。二年生白术需关注甲拌磷、氟虫腈、甲基异柳磷等农药的残留。Establish gas chromatography tandem mass spectrometry and ultra-high performance liquid chromatography tandem mass spectrometry methods for quantitative analysis,using both internal and external standard methods.Extract acetonitrile and concentrate it at low temperature using a parallel vacuum concentrator.Dilute and dissolve the sample with acetonitrile,and finally purify it through a hydrophilic and lipophilic equilibrium material solid-phase extraction column.Evaluate the contamination of the biennial atractylodes macrocephala traditional Chinese medicine by 33 prohibited pesticides.The results showed that the standard curves of the 33 prohibited pesticides were linear,with correlation coefficients greater than 0.99.The accuracy and repeatability recovery rates were between 61%and 118%.30 batches of biennial atractylodes macrocephala were detected with a detection rate of 66.6%,including Methionine,Flufipronil,and Methyl Isophos.Two year old atractylodes macrocephala needs to pay attention to the residues of pesticides such as phorate,fipronil,and methyl isocarbophos.
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