Determination Of Arsenice In Paediatric Qili San

Objective: In order to provide the data support for toxicological efficacy evaluation of pediatric Qili San,and accumulating data for the evaluation of traditional Chinese medicine which contains Realgar.Inductively coupled plasma mass spectrometry(ICP-MS)was used for the quantitative determination of total arsenic,soluble arsenic.And HPLC-ICP-MS was used for the quantitative determination of arsenite As(Ⅲ),arsenic As(Ⅴ),monomethyl arsenate(MMA),dimethyl arsenate(DMA)in pediatric Qili San with different pretreatment methods.Methods: Determination of the total arsenic in pediatric Qili San by ICP-MS: After the treatment with microwave digestion,samples were examined the Contents of total arsenic by ICP-MS,with Ge as internal standard.2.Determination of the soluble arsenic in pediatric Qili San by ICP-MS : Pretreating samples with artificial intestinal solution at 37 ℃ for 1 hour,the contents of soluble arsenic were examined by ICP-MS,with Ge as internal standard.3.Analysis the contents of arsenic As(Ⅲ),arsenate As(Ⅴ),monomethyl arsenate(MMA),and dimethyl arsenate(DMA)in pediatric Qili San by HPLC-ICP-MS: Pretreating samples with ultrasonic at 37 ℃ for 2 hours,contents of the four arsenic compounds above were examined by HPLC-ICP-MS.Results: 1.An ICP-MS method was developed for determing contents of the total arsenic in pediatric Qili San: The linear range was 0.2~10 ng/m L(r=0.9998),the limit of detection was 0.002 ng/m L,and the average recovery was 98.0~107%,RSD<3.6%(n=6).2.An ICP-MS method was developed for determing contents of the soluble arsenic in pediatric Qili San: The linear range was 0.2~10 ng/m L(r=0.9998),the limit of detection was 0.002 ng/m L,and the average recovery was 89.0~117%,RSD<3.0%(n=6).3.An HPLC-ICP-MS method was developed for determing contents of the four soluble arsenic in pediatric Qili San: The linear range was 0.2~10 ng/m L(r=0.9998),the limit of detection was 0.002 ng/m L,and the average recovery was 89.0~117%,RSD<3.0%(n=6).3.An HPLC-ICP-MS method was developed for determing contents of the four soluble arsenic in pediatric Qili San: The calibration curves were linear(r>0.999),respectively.The limits of detection were 0.03~0.07 ng/m L,and the average recoveries were 90.9~114.1%,RSD<6.0%(n=6).Conclusion(s): In this study,the method involving microwave digestion and ICP-MS analysis has been used for the determination of total arsenic and soluble arsenic in pediatric Qili San.It was found that the total arsenic in one of the samples reaches 35.2 g/kg and soluble arsenic in the range of 500~600mg/kg.The development of HPLC-ICP-MS method has been established for separation and simultaneous determination of As(III),As(V),MMA and DMA.And the method was proposed for speciation analysis of arsenic in 6 batches of pediatric Qili San.From this work,it was found that As(III)was the main chemical species in pediatric Qili San,more attention should be paid to this problem in the production of pediatric Qili San.The high performance of the methodology can be applied for the quality control and safety evaluation of the arsenic speciation analysis in pediatric Qili San,provides certain scientific basis for the evaluation of realgar Chinese patent medicine preparations,and provides data support for further toxicological efficacy evaluation of pediatric Qili San.