温州产山药中尿囊素及重金属含量的测定

Determination of Allantoin and Heavy Metal Content in Shanyao(Dioscoreae Rhizoma)from Wenzhou

目的:建立HPLC-亲水色谱法测定温山药中尿囊素的含量及ICP-MS法测定温山药中重金属的含量,并对收集到的30批次温山药样品进行检测。方法:尿囊素测定HPLC色谱条件:流动相为乙腈-水(70∶30),流速为0.5 mL/min,柱温为35℃,检测波长为210 nm,进样量为10μL;重金属测定:通过微波消解法对样品进行消解处理,采用内标法,用ICP-MS对30批次温山药中的铅、镉、砷、汞、铜同时进行测定。结果:尿囊素在测定范围内线性关系良好(r>0.9999),平均加样回收率为101.28%,RSD为1.67%;铅、镉、砷、汞、铜元素在各自范围内线性关系良好(r>0.99),平均加样回收率分别为91.56%%、91.25%、94.88%、95.67%、84.33%,检出限为0.0075~0.3318 ng/mL,30批次温山药样品重金属检测,结果均小于限度值。结论:本方法操作简便、灵敏、迅速、准确,可用于大样本量温山药样品中尿囊素及重金属的检测,为温山药的种植、生产及质量管控提供技术支撑。

Objective:To establish a HPLC-hydrophilic chromatography method for the determination of allantoin and ICP-MS method for the determination of heavy metals in Shanyao(Dioscoreae Rhizoma)from Wenzhou,and to detect 30 batches of Shanyao(Dioscoreae Rhizoma)samples collected.Methods:Determination of allantoin HPLC chromatographic conditions:mobile phase was acetonitrile-water(70∶30),flow rate was 0.5 mL/min,column temperature was 35℃,detection wavelength was 210 nm,injection volume was 10μL.Determination of heavy metals:the samples were digested by microwave digestion,and the internal standard method was used to simultaneously determine Pb,Cd,As,Hg and Cu in 30 batches of Shanyao(Dioscoreae Rhizoma)from Wenzhou by ICP-MS.Results:The linear relationship of allantoin in the determination range was good(r>0.9999),the average recovery rate was 101.28%,RSD was 1.67%.Pb,Cd,As,Hg and Cu have good linear relationship within their respective ranges(r>0.99).The average recovery rate was 91.56%,91.25%,94.88%,95.67%and 84.33%respectively,and the detection limit is 0.0075-0.3318 ng/mL.The heavy metal detection results of 30 batches of Shanyao(Dioscoreae Rhizoma)samples were less than the limit value.Conclusion:The method is simple,sensitive,rapid and accurate,which can be used for the detection of allantoin and heavy metals in large sample of Shanyao(Dioscoreae Rhizoma)samples,and provide technical support for the cultivation,production and quality control of Shanyao(Dioscoreae Rhizoma)from Wenzhou.