山西平顺县道地药材潞党参中重金属残留量分析
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篇名: 山西平顺县道地药材潞党参中重金属残留量分析
TITLE:
摘要: 目的:建立测定潞党参中铅(Pb)、镉(Cd)、铜(Cu)、砷(As)、汞(Hg)残留量的方法;并且评价山西平顺县潞党参的质量。方法:采用微波消解-电感耦合等离子体质谱法。扫描模式为动能歧视效应(KED)扫描模式,射频功率为1 550 W,采样深度为5.0 mm,等离子气(氩气)流量为16.0 L/min,氦气分压为0.1 mbar,氩气分压为0.6 mbar,真空度为5×10-8 mbar,分支涡轮泵转速为1 000 hz,采样锥孔径为1.0 mm,截取锥孔径为0.5 mm,雾化室温度为2.7 ℃,数据采集重复3次。结果:Pb、Cd、Cu、As、Hg检测质量浓度线性范围分别为0~20 ng/ml(r=0.999 3)、0~10 ng/ml(r=0.998 5)、0~250 ng/ml(r=0.998 8)、0~20 ng/ml(r=0.999 0)、0~1.0 ng/ml(r=0.997 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为95.80%~100.20%(RSD=1.85%)、94.50%~98.00%(RSD=1.26%)、98.52%~102.43%(RSD=1.60%)、94.90%~98.70%(RSD=2.29%)、96.00%~101.00%(RSD=1.84%),n均为6;检测限分别为0.021 0、0.003 4、0.043 7、0.115 6、0.005 6 ng/kg。山西平顺县潞党参基地药材中含有Pb、Cd、Cu、As,不含Hg,重金属总含量范围为7.185 2~12.558 0 mg/kg。结论:该方法操作简便,精密度、稳定性、重复性好,可用于潞党参中Pb、Cd、Cu、As、Hg残留量的测定;山西平顺县潞党参重金属残留均未超过国家及行业标准限量值。
ABSTRACT: OBJECTIVE: To establish a method for the residues determination of Pb, Cd, Cu, As and Hg in Codonopsis pilosula,and evaluate the quality evaluation of C. pilosula of Pingshun County in Shanxi province. METHODS: Microwave digestion-inductively coupled plasma mass spectrometry was adopted with KED scanning model, RF power was 1 550 W, sampling depth was 5.0 mm, plasma gas (argon) flow rate was 16.0 L/min, helium partial pressure was 0.1 mbar, argon gas was 0.6 mbar, the vacuum degree of 5×10-8 mbar, branch turbopump speed was 1 000 hz, sampling cone aperture was 1.0 mm, skimmer aperture was 0.5 mm, the spray chamber temperature was 2.7 ℃, the data collection was repeated 3 times. RESULTS: The linear range was 0-20 ng/ml for Pb (r=0.999 3), 0-10 ng/ml for Cd (r=0.998 5), 0-250 ng/ml for Cu (r=0.998 8), 0-20 ng/ml for As (r=0.999 0) and 0-1.0 ng/ml for Hg(r=0.997 9); RSDs of precision, stability and reproducibility tests were lower than 3.0%; recoveries were 95.80%-100.20% (RSD=1.85%,n=6), 94.50%-98.00% (RSD=1.26%,n=6), 98.52%-102.43% (RSD=1.60%,n=6), 94.90%-98.70%(RSD=2.29%,n=6) and 96.00%-101.00%(RSD=1.84%,n=6); the limits of detection were 0.021 0, 0.003 4, 0.043 7, 0.115 6 and 0.005 6 ng/kg, respectively. Pb, Cd, Cu, and As were detetcted,and Hg was not detected,the range of total contents was 7.185 2~12.558 0 mg/kg. CONCLUSIONS: The method is simple with good precision, stability and reproducibility, and can be used for the residues determination of Pb, Cd, Cu, As and Hg in C. pilosula; heavy metal residues in C. pilosula in Shanxi Pingshun county does not exceed limit values of national and industry standards
期刊: 2016年第27卷第24期
作者: 张德伟,胡娟娟,孟瑞丽,叶世碧,周浓
AUTHORS: ZHANG Dewei,HU Juanjuan,MENG Ruili,YE Shibi,ZHOU Nong
关键字: 平顺县;潞党参;重金属;残留量; 微波消解-电感耦合等离子体质谱法
KEYWORDS: Pingshun county; Codonopsis pilosula; Heavy metals; Residue; ICP-MS
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