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Preparation of Monoethyl Fumarate-Based Molecularly Imprinted Polymers and Their Application As SPE Sorbent for Enrichment of Scopolamine from Tropane Alkaloids

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Preparation of Monoethyl Fumarate-Based Molecularly Imprinted Polymers and Their Application As SPE Sorbent for Enrichment of Scopolamine from Tropane Alkaloids Electronic Supplementary Material (ESI) for RSC Advances. This journal is © The Royal Society of Chemistry 2019 Preparation of monoethyl fumarate-based molecularly imprinted polymers and their application as SPE sorbent for enrichment of scopolamine from tropane alkaloids Jie Zuo a, Xingyuan Zhang a*, Xinyu Li a, Zhiwei Li a, Zongren Li a, Honghong Li b, Wencheng Zhang b*. a CAS Key Laboratory of Soft Matter Chemistry, Department of Polymer Science and Engineering, University of Science and Technology of China, Hefei 230026, PR China. E-mail: [email protected]. b Engineering Research Center of Bio-Process of Ministry of Education, School of Food and Biological Engineering, Hefei University of Technology, Hefei, P. R. China. E-mail: [email protected]. 1. 1H NMR spectra The structure of synthetic functional monomer was identified using 1H NMR 1 spectra. As seen from Fig. S1, H NMR (400 MHz, DMSO-d6) δ: 1.21 (t, J=8 Hz, 3H), 4.14 (dd, J1=4 Hz, J2=8 Hz, 2H), 6.36 (q, J=12Hz, 2H), 12.97 (s, 1H), which proved mmaa-a-26 38000 HDO DMSO DMSO DMSO DMSO DMSO 36000 12.97 6.39 6.36 6.36 6.33 4.16 4.14 4.13 4.11 3.36 2.51 2.51 2.50 2.50 2.50 1.23 1.21 1.19 -0.00 34000 e 32000 30000 a O 6 28000 HO 4 b&c 26000 7 c 1 2 24000 b 22000 3 O 8 d 20000 O 9 d 18000 5 16000 H3C 10 DMSO 14000 e 12000 H2 O 10000 8000 6000 4000 a 2000 0 -2000 0.95 2.00 2.06 3.06 13.0 12.0 11.0 10.0 9.0 8.0 7.0 6.0 5.0 4.0 3.0 2.0 1.0 0.0 f1 (ppm) that MFMA had been successfully synthesized. Fig. S1. 1H NMR spectra of MFMA. 2. Method validation To verify the MISPE system integrated with HPLC, the favorable linear response was achieved within the scope of 8.0–4.0×104 μg L−1. with R2 of 0.9982. Furthermore, limit of detection (LOD), which stands for minimum detectable concentration, was 2.2 μg L−1. Limit of quantification (LOQ) that represents smallest amount of analyte measured with reasonable accuracy was 6.5 μg L−1. To evaluate the precision of the MISPE for scopolamine analysis, three Hindu Datura samples each added with scopolamine (0.1 mg L−1) were researched by MISPE system to obtain the relative standard deviation (RSD) of 2.4%. In order to further evaluate the MISPE system, the established a non-aqueous SPE method using silica based strong cation exchange (SCX)37 (SCX-SPE) were applied to study the Hindu Datura and Belladonna samples. The data summarized in Table S1 exhibited that the recovery of MFMA-MISPE method (96.0–106.0%) was higher than that of SCX-SPE method (78.0-85.0%). The above results indicate that the MFMA- MISPE method is more advantageous than the SCX-SPE method in enrichment of scopolamine from plants samples. Therefore, the MFMA-MISPE system integrated with HPLC is more desirable for the extraction and detection of scopolamine in the mixture of tropane alkaloids. Table S1. Comparison of the MFMA-MISPE method with SCX-SPE method. Detected (μg L-1) Recovery (%) RSD (%) Added Samples (μg L-1) MFMA-MISPE SCX-SPE MFMA-MISPE SCX-SPE MFMA-MISPE SCX-SPE - NDa ND - - - - Hindu Datura 50.0 51.0 45.0 102.0 85.0 3.4 4.5 100.0 96.0 80.0 96.0 80.0 2.7 5.2 - ND ND - - - - Belladonna 50.0 53.0 41.0 106.0 82.0 4.1 6.7 100.0 99.0 78.0 99.0 78.0 3.5 5.5 a ND is not detected.
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