RESUMO
OBJECTIVE:To establish a method for simultaneous determination of 18 toxic elements from 10 ingredients of Modified xiaoyao formula and their extracts,and to study transport rates of above elements. METHODS:Microwave digestion-in-ductively coupled plasma mass (ICP-MS) was used to determine above elements. Radio-frequency power was 1.50 kW,atomiza-tion pressure was 720 kPa,sampling depth was 7 mm,plasma gas flow rate was 15.0 L/min,carrier gas flow rate was 1.00 L/min, spray chamber temperature was 2℃,He flow rate was 4.5 mL/min under collision mode,measurement points/peak was 3,data ac-quisition mode was jump mode. RESULTS:The linear ranges of As,Pb,Cu,Hg,Cd,Mo,V,Cr,Mn,Fe,Ni,Zn,Ru,Rh, Pd,Os,Ir,Pt was 0-500.17 ppb(r was 0.9994-09999);LOD was 0.0004-5.3410 ng/g;RSD of repeatability tests was all lower than 5.0%;average recoveries were 82.0%-117.9%(RSD=0.2%-5.7%,n=9). Ru,Rh,Pd,Os,Ir,Pt,Hg had not been detect-ed. The transfer rates of 11 metals in the extracts ranged 1.46%-31.90%. CONCLUSIONS:The method is simple,precise,stable and repeatable,and can be used for simultaneous determination of 18 toxic elements in 10 ingredients of Modified xiaoyao formula and their extracts. The contents of toxic elements are decreased during the preparation of Modified xiaoyao formula extract to guar-antee the safety of drug use to certain extent.
RESUMO
Objective To provide a proper concentration of Internal Standard Solution by comparing five different degrees to the simultaneous analysis of 10 metals including V,Cr,Mn,Fe,Ni,Cu,As,Cd,Pb and Hg in Cardeniajasminoides.Method An Inductively Coupled Plasma-Mass Spectrometry method with Microwave-Assisted Digestion was developed with10,50,200,500,1 000 μg/L of Ge,In,Bi as internal standard.Result The degree of 500 μg/L concentration of internal stand solution can both correct the matrix effect and alleviate the contamination as the 1 000 μg/L.Conclusion With excellent detection limits,high sensitivity and wide linear range,the 500 μg/L internal standard may serve as reference in the determination of elements in other traditional Chinese medicine (TCM).