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、0.2~4 ng/mL(r均大于0.997);检测限分别为0.0411、0.0132、0.0573、0.0090、0.0054 ng/mL,定量限分别为0.1370、0.0440、0.1910、0.0300、0.0180 ng/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(28 h)的RSD均小于5%,Hg元素稳定性试验(28 h)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、0.0019~0.0054 mg/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。
OBJECTIVE:To establish 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 0.0411,0.0132,0.0573,0.0090,0.0054 ng/mL,respectively.The limits of quantification(LOQs)were 0.1370,0.0440,0.1910,0.0300,0.0180 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 0.1910-1.5276,0.0025-0.0474,0.0341-1.5490,0.0015-0.0788 and 0.0019-0.0054 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.
作者
彭双
杨海源
张敏娟
魏文芝
PENG Shuang;YANGHaiyuan;ZHANG Minjuan;WEI Wenzhi(Qinghai Provincial Drug Inspection and Testing Institute,Xining 810016,China;NMPA Key Laboratory for Quality Control of TCM(Tibetan Medicine),Xining 810016,China;Qinghai Provincial Key Laboratory of Modernization of Traditional Chinese and Tibetan Medicine,Xining 810016,China)
出处
《中国药房》
CAS
北大核心
2021年第18期2218-2222,共5页
China Pharmacy
基金
国家药品抽检计划项目(No.国药监药管[2020]1号)。
关键词
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
Pediatric paracetamol artificial cow-bezoar and chlorphenamine maleate granules
ICP-MS
Heavy metals
Harmful elements
