微波消解-ICP/MS法测定乙交酯丙交酯共聚物(25∶75)中锡元素

目的 ：考察乙交酯丙交酯共聚物(25∶ 75)中催化剂锡的残留量。 方法：采用微波消解-电感耦合等离子体质谱法测定乙交酯丙交酯共聚物(PLGA)中锡的量。射频功率：1.5 kW；载气流量：0.82 L·min^-1；辅助气流量：0.21 L·min^-1；采样深度：8.5 mm。 结果：锡元素线性关系良好，回归方程为Y=0.2848X-0.03583，相关系数为0.9999，重复性RSD为0.65%，加标回收率为98%~102%，检出限为0.13 ng·g^-1，定量限为0.42 ng·g^-1。 结论：本文建立的方法样品用量少，操作简便，分析速度快，经方法学验证满足锡残留量的检测。

Objective: To investigate the residual amount of catalyst tin in poly(lactide-co-glycolide)(25∶ 75). Methods: The microwave digestion-ICP/MS was used to determine the amount of tin in poly(lactide-co-glycolide)(PLGA).The radio-frequency power was 1.5 kW,the flow rate of carrier gas was 0.82 L·min^-1,the auxiliary gas flow was 0.21 L·min^-1,the sampling depth was 8.5 mm. Results: Linear relationship of tin was good,the regression equation was Y=0.2848X-0.03583,the correlation coefficient was 0.9999,the repetitive RSD was 0.65%,the recovery rate was 98%-102%,the detection limit was 0.13 ng·g^-1,the limit of quantification was 0.42 ng·g^-1. Conclusion: The microwave digestion-ICP/MS method has a high sensitivity,a strong specificity,a fast analysis speed,and it only requires a small amount of sample which can support the determination of tin in PLGA.

[1] Bilati U，Alleman E，Doellker E.Poly(D,L-lactide-co-glycolide)protein loaded nanoparticles prepared by the double emulsion method-processing and formulation issues for enhanced entrapment efficiency[J].J Microencapsul,2005,22(2):205
[2] WANG Yu（王玉），WANG Dong-kai(王东凯)，SUN Nian（孙念）.Nano and micro technologies for delivering macromolecular therapeutics using poly(lactide-co-glycolide)(聚丙交酯乙交酯共聚物作为大分子药物载体的纳米及微米技术研究进展)[J].Chin J Pharm（中国药剂学杂志），2009,7（3）：20
[3] ZHANG Xia(张霞)，LIU Wen-jie(刘文杰).The toxicity and determination of tin(锡的毒性及测定). J Hyg Res(卫生研究)，2002,31(4):322
[4] YANG Li（杨莉），LUAN Han-sen（栾瀚森），XU Feng-lan（徐凤兰），et al.Removal of organotin during purification process of poly(lactic-co-glycolic acid)(乙交酯-丙交酯共聚物精制过程中有机锡的去除方法)[J].Chin J Pharm（中国医药工业杂志），2013,44（3）：235
[5] DONG Shun-ling(董顺玲).Determination of Cu,Cr,Cd,Pb,As,Sb,Sn and Hg in Ejiao by AAS(原子吸收光谱法测定中成药阿胶中铜、铬、镉、铅、砷、锑、锡和汞)[J].Spectrosc Spect Anal (光谱学与光谱分析)，1996，12（16）:91
[6]JIN Bo(金波)，MA Chen(马辰).Simultaneous determination of tin and bismuth in medicinal and edible Chinese medicinal materials by hydride generation-atomic fluorescence spetremetry(氢化物发生-原子荧光法同时测定药食同源药材中痕量锡和铋)[J].Chin J Health Lab Technol(中国卫生检验杂志)，2011,2（21）:311
[7] GB/T 5009.16-2003，Determination of Tin in Foods（食品中锡的测定）[S].2003