ICP-MS法测定小儿氨酚黄那敏颗粒中重金属及有害元素的含量
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篇名: ICP-MS法测定小儿氨酚黄那敏颗粒中重金属及有害元素的含量
TITLE: Determination of the Contents of Heavy Metals and Harmful Elements in Pediatric ,Paracetamol,Atificial Cow- bezoar and Chlorphenamine Maleate Granules by ICP-MS
摘要: 目的:建立同时测定小儿氨酚黄那敏颗粒中重金属铅(Pb)、镉(Cd)、铜(Cu)、汞(Hg)以及有害元素砷(As)含量的方法。方法:样品经微波消解后,以锗、铟、铋元素为内标,采用电感耦合等离子体质谱法(ICP-MS)测定。结果:Pb、As、Cu、Cd、Hg元素检测质量浓度的线性范围分别为1~20、0.5~10、5~100、0.5~10、0.2~4ng/mL(r均大于0.997);检测限分别为0.0411、0.0132、0.0573、0.0090、0.0054ng/mL,定量限分别为0.1370、0.0440、0.1910、0.0300、0.0180ng/mL;精密度、重复性试验的RSD均小于6%,Pb、As、Cu、Cd元素稳定性试验(28h)的RSD均小于5%,Hg元素稳定性试验(28h)的RSD小于7%;平均加样回收率分别为89.44%(RSD=5.87%,n=9)、99.56%(RSD=5.46%,n=9)、96.12%(RSD=4.62%,n=9)、105.82%(RSD=2.80%,n=9)、90.23%(RSD=3.59%,n=9)。63批样品中,Pb、As、Cu、Cd、Hg等5种元素均有检出,含量分别为0.1910~1.5276、0.0025~0.0474、0.0341~1.5490、0.0015~0.0788、0.0019~0.0054mg/kg。结论:该方法操作简便、灵敏、准确,可用于同时测定小儿氨酚黄那敏颗粒中5种元素的含量。
ABSTRACT: OBJECTIVE:To es tablish a method for the content determination of heavy metals [lead (Pb),cadmium(Cd), copper (Cu), mercury (Hg)] and harmful elements [arsenic (As)] in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules. METHODS :The samples were conducted pretreatment by microwave digestion instrument and determined by inductively coupled plasma mass spectrometry (ICP-MS)using elements germanium ,indium,bismuth as internal standard. RESULTS :The linear ranges of Pb ,As,Cu,Cd and Hg were 1-20,0.5-10,5-100,0.5-10 and 0.2-4 ng/mL, respectively (all r>0.997). The limits of detection (LODs) were 0.041 1,0.013 2,0.057 3,0.009 0,0.005 4 ng/mL, respectively. The limits of quantification (LOQs)were 0.137 0,0.044 0,0.191 0,0.030 0,0.018 0 ng/mL,respectively. RSDs of precision and repeatability tests were all less than 6%. RSDs of stability tests (28 h)of Pb ,As,Cu and Cd were all less than 5%, and that of stability test (28 h)of Hg was less than 7%. The average recoveries were 89.44%(RSD=5.87%,n=9),99.56% (RSD=5.46% ,n=9),96.12%(RSD=4.62% ,n=9),105.82%(RSD=2.80% ,n=9)and 90.23%(RSD=3.59% ,n=9), respectively. Five elements were all detected in 63 batches of samples ,and the contents of them were 0.191 0-1.527 6,0.002 5- 0.047 4,0.034 1-1.549 0,0.001 5-0.078 8 and 0.001 9-0.005 4 mg/kg,respectively. CONCLUSIONS :The method is simple , sensitive and accurate. It is suitable for simultaneous determination of 5 elements in Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules.
期刊: 2021年第32卷第18期
作者: 彭双,杨海源,张敏娟,魏文芝
AUTHORS: PENG Shuang ,YANG Haiyuan ,ZHANG Minjuan ,WEI Wenzhi
关键字: 小儿氨酚黄那敏颗粒;电感耦合等离子体质谱法;重金属;有害元素
KEYWORDS: Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules ;ICP-MS;Heavy metals ;
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