电感耦合等离子体质谱法测定“十大晋药”中5种有害元素及风险评估

Determination of Five Harmful Elements in Ten Famous Herbal Drugs in Shanxi by ICP-MS and Risk Assessment

目的 建立测定“十大晋药”黄芪、党参、连翘、远志、柴胡、黄芩、酸枣仁、苦参、山楂、桃仁中铅(Pb)、砷(As)、镉(Cd)、汞(Hg)、铜(Cu)5种有害元素含量的电感耦合等离子体质谱(ICP-MS)法。方法 采用微波消解法处理样品,以锗(^(72)Ge)、铟(^(115)In)、铋(^(209)Bi)为内标。采用ICP-MS法测定,射频功率为1 200 W,采用碰撞模式,碰撞气为氦气,载气为氩气,载气流速为0.70 L/min,等离子体气体流速为9.00 L/min,泵速为0.3 r/s。结果 Pb质量浓度在0~50 ng/mL,As质量浓度在0~50 ng/mL,Cd质量浓度在0~10 ng/mL,Hg质量浓度在0~5 ng/mL,Cu质量浓度在0~200 ng/mL范围内与响应值线性关系良好(R^(2)≥0.999 4);检测限分别为0.20,0.20,0.02,0.01,0.50 ng/mL,定量限分别为0.70,0.70,0.06,0.03,1.70 ng/mL;回收率分别为94.94%,81.30%,88.30%,85.00%,93.81%,RSD分别为2.01%,1.63%,1.32%,1.83%,1.12%(n=6);重复性试验结果的RSD为0.92%~2.31%(n=6);精密度试验结果的RSD为0.81%~3.81%(n=6)。Pb,As,Cd,Hg,Cu有害元素的风险评估靶标危害指数(THQ)均小于1。结论 该方法简便、高效,可为“十大晋药”中有害元素分析方法的建立与评估提供参考。

Objective To establish an inductively coupled plasma mass spectrometry (ICP-MS) method for the content determination of five harmful elements[lead (Pb),arsenic (As),cadmium (Cd),mercury (Hg),and copper (Cu)]in ten famous herbal drugs in Shanxi,such as Astragali Radix,Codonopsis Radix,Forsythiae Fructus,Polygalae Radix,Bupleuri Radix,Scutellariae Radix,Ziziphi Spinosae Semen,Sophorae Flavescentis Radix,Crataegi Fructus,Persicae Semen.Methods The samples were pretreated by microwave digestion method,with germanium(^(72)Ge),indium(^(115)In),and bismuth(^(209)Bi)as internal standards.The ICP-MS method was adopted with the radio frequency (RF) power of 1 200 W,the collision mode was adopted,the collision gas was helium,the carrier gas was argon,the carrier gas flow rate was 0.70 L/min,the plasma gas flow rate was 9.00 L/min,and the pump speed was 0.3 r/s.Results The linear ranges of Pb,As,Cd,Hg,and Cu were 0-50 ng/mL,0-50 ng/mL,0-10 ng/mL,0-5 ng/mL,and 0-200 ng/mL (R^(2)≥0.999 4),respectively.The limits of detection (LOD) were 0.20,0.20,0.02,0.01,and 0.50 ng/mL,respectively.The limits of quantification (LOQ) were 0.70,0.70,0.06,0.03,and 1.70 ng/mL,respectively.The recovery rates of Pb,As,Cd,Hg,and Cu were 94.94%,81.30%,88.30%,85.00%,and 93.81%,with RSDs of 2.01%,1.63%,1.32%,1.83%,and 1.12%(n=6),respectively.The RSD of the repeatability test result was in the range of 0.92%-2.31%(n=6).The RSD of the precision test result was in the range of 0.81%-3.81%(n=6).The target hazard quotients (THQ)for risk assessment of harmful elements such as Pb,As,Cd,Hg,and Cu were all lower than 1.Conclusion The method is simple and sensitive,which can provide a reference for the establishment and evaluation of analysis methods for harmful elements in the ten famous herbal drugs in Shanxi.