冬凌草饮片中外源性有害物质残留检测OA
Residues of Exogenous Harmful Substances in Rabdosiae Rubescentis Herba Pieces
目的 建立检测冬凌草饮片中外源性有害物质(含重金属及有害元素、植物生长调节剂)残留的方法.方法 采用微波消解法对样品进行前处理.采用电感耦合等离子体质谱(ICP-MS)法测定样品中铅(Pb)、镉(Cd)、砷(As)、汞(Hg)、铜(Cu)5 种重金属及有害元素的含量.采用超高效液相色谱串联质谱(UPLC-MS/MS)法测定莠去津、仲丁灵、矮壮素、坐果安、氯苯胺灵、增产胺、胺鲜酯、1,3-二苯基脲、吲熟酯、氟节胺、呋嘧醇、糠氨基嘌呤、抗倒胺、甲哌鎓、烯腺嘌呤、萘乙酰胺、多效唑、吡啶醇、反式玉米素、抑芽唑、烯效唑、6-苄氨基嘌呤、氯吡脲、噻苯隆 24 种植物生长调节剂的残留量.结果 各重金属及有害元素、植物生长调节剂均在相应质量浓度范围内与待测元素/内标元素仪器响应值或峰面积线性关系良好(r>0.990,n=6),检测限分别为 0.000 2～0.001 0 mg/kg、0.01～0.10 mg/kg,定量限分别为 0.000 5～0.003 5 mg/kg、0.03～0.30 mg/kg;精密度、稳定性试验结果的 RSD 均小于 5.0%;平均加样回收率分别为 90.18%～105.12%(RSD 为 0.59%～2.22%)、75.31%～90.82%(RSD 为 0.31%～4.61%)(n=6).27 批样品中重金属均有检出,其中4批Pb超标,1批Hg超标,1批Cd超标;检出5批吡啶醇残留,含量为0.012～0.096 mg/kg,但均低于定量限(0.15mg/kg).结论 所建方法操作简单、结果准确,可用于冬凌草饮片中外源性有害物质的检测.
Objective To establish a method for the determination of exogenous harmful substances(including heavy metals and harmful elements,as well as plant growth regulators)in Rabdosiae Rubescentis Herba pieces.Methods The samples were pretreated by microwave digestion.Inductively coupled plasma mass spectrometry(ICP-MS)was used to determine the contents of five heavy metals and harmful elements,including lead(Pb),cadmium(Cd),arsenic(As),mercury(Hg)and copper(Cu)in the samples.Ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was used to determine the residues of 24 plant growth regulators,including atrazine,butralin,chlormequat chloride,fruitone CPA,chlorpropham,guayule,2-diethylaminoethyl hexanoate,1,3-diphenylurea,ethychlozate,flumetralin,flurprimidol,kinetin,inabenfide,mepiquat,enadenine,naphthylacetamide,paclobutrazol,pyripropanol,trans-zeatin,triapenthenol,uniconazole,6-benzylaminopurine,forchlorfenuron and thidiazuron.Results All heavy metals and harmful elements,as well as plant growth regulators showed good linear relationships with the instrument response value of analyte/internal standard element or peak area in the corresponding concentration ranges(r>0.990,n=6).The limits of detection were 0.000 2-0.001 0 mg/kg and 0.01-0.10 mg/kg,respectively;the limits of quantitation were 0.000 5-0.003 5 mg/kg and 0.03-0.30 mg/kg,respectively.The RSDs of precision and stability tests were all lower than 5.0%.The average recoveries were 90.18%-105.12%(with RSDs of 0.59%-2.22%)and 75.31%-90.82%(with RSDs of 0.31%-4.61%),respectively(n=6).Heavy metals were detected in all 27 batches of samples,among which four batches exceeded the limit of Pb,one batch exceeded the limit of Hg and one batch exceeded the limit of Cd.Pyripropanoll residues were detected in five batches of samples,the contents range was 0.012-0.096 mg/kg,all of which were lower than the limit of quantitation(0.15 mg/kg).Conclusion The established method is simple and accurate,and can be used for the control of exogenous harmful substances in Rabdosiae Rubescentis Herba pieces.
杨秋红;李珊;黄霞;李海燕;刘亚楠;王海波
河南省药品医疗器械检验院·河南省中药质量控制工程研究中心,河南 郑州 450018河南省药品医疗器械检验院·河南省中药质量控制工程研究中心,河南 郑州 450018河南省药品医疗器械检验院·河南省中药质量控制工程研究中心,河南 郑州 450018河南省药品医疗器械检验院·河南省中药质量控制工程研究中心,河南 郑州 450018河南省药品医疗器械检验院·河南省中药质量控制工程研究中心,河南 郑州 450018河南省药品医疗器械检验院·河南省中药质量控制工程研究中心,河南 郑州 450018
医药卫生
冬凌草饮片电感耦合等离子体质谱法超高效液相色谱串联质谱法重金属有害元素植物生长调节剂
Rabdosiae Rubescentis Herba piecesinductively coupled plasma mass spectrometryultra-performance liquid chromatography-tandem mass spectrometryheavy metalharmful elementplant growth regulator
《中国药业》 2026 (8)
75-80,6
国家药品监督管理局药品监管科学体系建设重点项目[RS2024Z006]国家药品监督管理局中药材及饮片质量控制重点实验室项目[ZZ202303]河南省市场监督管理局科技计划项目[HNSCJGK202424].
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