Efficient synthesis of ionic triblock copolyesters and facile access to charge-reversal hybrid micells Shaohua Wu,a,b Liuchun Zheng,*,a Wen Zhou,c Chuncheng Li,*,a Yaonan Xiao,a and Wenxiang Zhua a Beijing national laboratory for Molecular Sciences, Key Laboratory of Engineering Plastics, Institute of Chemistry, Chinese Academy of Sciences (ICCAS), Beijing, PR China; Tel: +86-10-62562292; Fax: +86-10-62562292. E-mail: hubeizlc@iccas.ac.cn; lichch@iccas.ac.cn b University c Institute of the Chinese Academy of Sciences, Beijing 100049, PR China of Chemical Defence, Beijing, 102205, People’s Republic of China Determination of the content of Nile red loaded in the hybrid micelles The solution of Nile red-loaded hybrid micelles was lyophilized and then the dried micelles were dissolved in DMF. The UV absorbance at 545 nm was measured to determine the Nile red concentration on the basis of the standard curve of the UV absorbance of Nile red in DMF solution. The loading content (LC) and loading efficiency (LE) of Nile red in the hybrid micelles were calculated according to the following equations: LC (wt%) = 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑙𝑜𝑎𝑑𝑒𝑑 𝑑𝑦𝑒 × 100% 𝑡𝑜𝑡𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑜𝑙𝑦𝑚𝑒𝑟 𝑎𝑛𝑑 𝑙𝑜𝑎𝑑𝑒𝑑 𝑑𝑦𝑒 LE (%) = 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑙𝑜𝑎𝑑𝑒𝑑 𝑑𝑦𝑒 × 100% 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑑𝑦𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑 Figure S1. 1H NMR spectrum of prepared dihydroxyl-terminated PBF macroinitiator. Figure S2. GPC traces of dihydroxyl-terminated PBF macroinitiator and PCL-b-PBF-b-PCL triblock copolyesters. 2 Figure S3. DLS and TEM results of cationic micelles. Figure S4. Fluorescence emission spectra of Nile red in cationic micelles of varying concentrations (a) and plot of the emission intensity at 610 nm as a function of concentration of micelles (b). 3