摘要
目的优化中成药丸剂中痕量铅含量的快速检测方法,探讨其在市售中成药铅含量检测中的应用。方法采用电热消解法消解样品,原子荧光光谱法进行测定。通过正交实验设计优化实验条件,确定仪器最佳测定参数、载流浓度以及还原剂体系浓度配比,建立与优化痕量铅的电热消解-氢化物发生-原子荧光光谱法,并应用于市售中成药的检测。结果电热消解-氢化物发生-原子荧光光谱法中铅浓度在0~20μg/L,浓度范围内线性关系良好,回归方程为y=330.572x+65.427,相关系数为0.9998,相对标准偏差(RSD)为0.788%,检出限为0.0352μg/L,加标回收率为92.3%~104.4%。使用该法检测市售中成药铅含量,牛黄解毒片、乌鸡白凤丸和六味地黄丸中均有检出,介于0.106~0.300 mg/kg,含量在限量标准之内。结论以电热消解法消解样品,以3.5%HNO3为载流,以2%KBH4-3%KOH-1.2%K3Fe(CN)6-0.1%H3BO3为还原体系,优化了中成药痕量铅检测的电热消解-氢化物发生-原子荧光光谱法,该法准确可靠,灵敏度高,干扰小,简便快速,适用于中成药丸剂痕量铅的快速测定;市售中成药牛黄解毒片、乌鸡白凤丸和六味地黄丸中铅含量在限量标准之内。
Objective To optimize rapid determination of trace lead in pilled Chinese patent medicines,and to validate its use for measurement of lead content in commercial Chinese patent medicines.Methods The study samples were processed by electrothermal digestion,and then tested by atomic fluorescence spectrometry(AFS).The experimental conditions,including the instrumentation parameters,the carrier concentration and the concentration ratio of the reducing agent system,were optimized through orthogonal experimental design.Thereby,an approch of trace lead measurement via electrothermal digestion-hydride generation-AFS was optimized and established,which was subsequently used in testing of commercial Chinese patent medicines.Results The lead content measured via electrothermal digestion-hydride generation-AFS was 0-20μg/L,showing good linear relationship within the concentration range.The regression equation was formulated as y=330.572x+65.427,with a correlation coefficient of 0.9998,a relative standard deviation(RSD)of 0.788%,a detection limit of 0.0352μg/L,and a spiked recovery rate of 92.3%-104.4%.Using this approach for testing of commercially available Chinese patent medicines,trace lead was detectable in Niuhuang Jiedu Wan,Wuji Baifeng Wan and Liuwei Dihuang Wan,ranging from 0.106 to 0.300 mg/kg which was within the allowable limits by Chinese Pharmacopedia.Conclusion We established an optimal approach for measurement of trace lead in Chinese patent medicines through electrothermal digestion-hydride generation-AFS,which involves electrothermal digestion for sample processing,3.5%HNO3 as the carrier,and 2%KBH4-3%KOH-1.2%K3Fe(CN)6-0.1%H3BO3 as the reduction system.This approach appears accurate,reliable,highly sensitive,less interferenced,easy and quick to use,and therefore is suitable for rapid determination of trace lead in pilled Chinese patent medicines.According to our measurement,the lead content in commercial Chinese patent medicines Niuhuang Jiedu Wan,Wuji Baifeng Wan and Liuwei Dihuang Wan is within the allowable limits.
作者
高林英
常雪
边霞
刘桂英
杨秀娟
Gao Linying;Chang Xue;Bian Xia;Liu Guiying;Yang Xiujuan(School of Public Health Shanxi Medical University,Taiyuan 030001,China)
出处
《中国药物与临床》
CAS
2021年第1期11-13,共3页
Chinese Remedies & Clinics
基金
山西省青年科技研究基金(201801D221404)
山西医科大学大学生创新创业训练项目(20170332)。
关键词
中成药丸剂
铅
原子荧光光谱法
Pilled Chinese patent medicine
Lead
Atomic fluorescence spectrometry
