原子吸收法测定药用硅酸钙中铅的含量

Determination of Lead in Pharmaceutical Calcium Silicate by Atomic Absorption Spectrometry

建立原子吸收法测定药用辅料硅酸钙中铅的含量。收集国内外不同厂家不同批次的硅酸钙样品,参照中国药典铅、镉、砷、汞、铜测定法(通则2321第一法),以及美国药典对硅酸钙中铅含量的测定方法,以石墨炉为原子化器,在波长283. 3 nm处测定硅酸钙中铅的含量。不同厂家的7批硅酸钙样品中铅的含量均符合要求,均不超过5 mg/kg,其中铅的含量在5~80 ng/m L浓度范围内成良好线性关系,线性方程为y=0. 008 9x+0. 056 6,r=0. 995 2,精密度良好,RSD为18. 61%,加样回收率均在85%~115%的范围内,检出限为0. 066 3 ng/m L。该方法灵敏度高,专属性强,可以准确地测定硅酸钙中铅的含量,为提高药用辅料硅酸钙的质量标准提供研究思路。

To establish the atomic absorption method for determination of lead in calcium silicate as a pharmaceutical excipient,to improve the quality standard of calcium silicate for pharmaceutical excipients,and to make the use of pharmaceutical excipients safer,different samples of calcium silicate samples from different manufacturers at home and abroad were collected.The characteristics of high-pressure closed digestion and rapid microwave heating were used to digest the calcium silicate samples.The acid dosage was small,the digestion was complete,and the digestion process was completed.The tested samples are based on the 2015 edition of the Chinese Pharmacopoeia,(the lead,cadmium,arsenic,mercury,and copper assays)(General Law 2321,First Law),and the US Pharmacopoeia’s method for determining the lead content in calcium silicate.The method of determining the content of lead was established.The content of lead in calcium silicate was measured at a wavelength of 283.3 nm using a graphite furnace as an atomizer.The difference in the content of lead calcium silicate between different domestic and foreign pharmaceutical materials was compared.The lead content of 7 batches of calcium silicate samples from different manufacturers met the requirements,no more than5 mg/kg,and the lead content in the concentration range of 5~80 ng/m L became a good linear relationship.The linear equation is y=0.008 9 x+0.056 6,r=0.995 2,the precision is good,the RSD is 18.61%,the recovery rate of the sample is in the range of85%~115%,and the detection limit is 0.066 3 ng/m L.The method has low detection limit,high sensitivity,strong specificity and easy operation,and can accurately determine the content of lead in calcium silicate,which provides a simple and popular method for the quality control of calcium silicate,to provide research ideas for improving the quality standards of pharmaceutical adjuvant calcium silicate.