药用玻璃容器中砷、锑、铅、镉浸出量测定方法的研究

目的建立新的药用玻璃容器中砷、锑、铅、镉浸出量的测定方法。方法采用原子荧光光谱法同时测定药用玻璃容器中砷和锑的浸出量，采用石墨炉原子吸收光谱法测定铅、镉的浸出量。结果砷在0～10μg·L^-1范围内线性良好，r=0．9996，检出限为0．0449μg·L^-1，平均回收率为101．3％，RSD=0．7％（n=9）；锑在0～10μg·L^-1范围内线性良好，r=0．9997，检出限为0．0612μg·L^-1，平均回收率为93．9％，RSD=1．9％（n=9）；铅在0～50μg·L^-1范围内线性良好，r=0．9962，检出限为0．6557μg·L^-1，平均回收率为106．0％，RSD=6．1％（n=9）；镉在0～5μg·L^-1范围内线性良好，r=0．9987，检出限为0．1000μg·L^-1，平均回收率为106．8％，RSD=2．5％（n=9）。结论新建方法符合方法验证要求，能对药用玻璃容器中砷、锑、铅、镉的浸出量进行检测。

Study on A Method for Measurement of As,Sb, Pb,Cd Extraction in Pharmaceutical Glass Containers

Objective To establish a new method for measurement of As, Sb, Pb, Cd extraction in pharmaceutical glass containers. Methods The As and Sh extraction was measured in pharmaceutical glass containers by atomic fluorescence spectrometry simultaneously. The Pb and Cd extraction was determined by graphite furnace atomic absorption spectrometry. Results The As extraction showed good linearity in the range of 0-10 μg·L^-1 , r=0. 9996. Its detection limit was O. 0449 μg·L^-1 and the average recovery was 101.3%, RSD=0.7% （n=9）. The Sb extraction showed good linearity in the range of 0-10 μg·L^-1, r=0. 9997. Its detection limit was 0. 0612 μg·L^-1 and the average recovery was 93.9%, RSD=1.9% （n=9）.The Pb extraction showed good linearity in the range of 0-50 μg·L^-1, r=0. 9962. Its detection limit was 0. 6557 μg·L^-1 and the average recovery was 106.0%, RSD=6.1% （n=9）. The Cd extraction showed good linearity in the range of 0-5 μg·L^-1 , r= 0. 9987. Its detection limit was 0. 1000 μg·L^-1 and the average recovery was 106.8%, RSD=2.5% （n=9）. Conclusion The method is in accordance with the requirements of the methodology validation. It can be used for detection of As, Sh, Pb, Cd extraction in pharmaceutical glass containers.