Department of Chemistry, Faculty of Sciences, Shahrekord University, P.O. Box 115, Shahrekord, Iran.
Chemistry & Chemical Engineering Research Center of Iran (CCERCI), P.O. Box 14335-186, Tehran, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Oct 1;1182:122941. doi: 10.1016/j.jchromb.2021.122941. Epub 2021 Sep 11.
To ascertain thymol and carvacrol in pharmaceutical syrups, a valid and effective magnetic molecular imprinted polymer dispersive solid phase microextraction (MMIP-DSPME) process was developed in this study, which was in combination with a high performance liquid chromatography-ultra violet (HPLC-UV) technique for the assessment of thymol and carvacrol separation and pre-concentration. Contact time, eluent kind and volume, pH, the mass of the MMIP were all taken into consideration as key factors. Design expert and multi-objective response surface methodology (RSM) were used to optimize these variables. The mass of the MMIP, sample pH, eluent kind, time of sorption, the volume of eluent, and time of elution were 10 mg, 6, acetonitrile, 28 min, 200 µL, and 5.5 min, respectively, for the maximum extraction recovery of the analytes. The limit of detection (LOD) was 0.042 ng mL at the optimal conditions, while the value for the limit of quantification (LOQ) was 0.140 ng mL. At the optimized conditions for thymol and carvacrol, the suggested MMIP sorbent had sorption capacities of 64.1 and 72.6 mg g, respectively. Furthermore, for triplicate measurements, the linear dynamic range (LDR) was 0.40-5000 ng mL, and the method's accuracy (RSD %) was 6.26%. The saturation magnetization for the MMIP was 19.0 emu g obtained by VSM, allowing the sorbent to be separated quickly. The sorption experiments confirmed the large sorption capacity of the MMIP for thymol and carvacrol, as well as its homogeneous binding sites. The extraction recovery for thymol and carvacrol was 96.9-103.8% and 96.6-105.4%, respectively, at all spiked amounts (20, 100, 200, and 500 ng mL). The findings of seven desorption-regeneration cycles using MMIP demonstrated the high stability of the sorbent. The MMIP revealed a particular behavior of sorption for thymol and carvacrol, implying a selective, simple, effective, and flexible analytical method.
为了在药物糖浆中测定麝香草酚和香芹酚的含量，本研究建立了一种有效的磁性分子印迹聚合物分散固相微萃取（MMIP-DSPME）方法，该方法结合高效液相色谱-紫外（HPLC-UV）技术，用于评估麝香草酚和香芹酚的分离和预浓缩。考察了接触时间、洗脱剂种类和体积、pH 值、MMIP 质量等关键因素。采用设计专家和多目标响应面法（RSM）对这些变量进行了优化。最佳萃取条件为：MMIP 质量 10mg、样品 pH 值 6、洗脱剂种类为乙腈、吸附时间 28min、洗脱剂体积 200μL、洗脱时间 5.5min。在此最佳条件下，分析物的最大萃取回收率分别为 64.1 和 72.6mg/g。在最佳条件下，麝香草酚和香芹酚的检测限（LOD）分别为 0.042ng/mL 和 0.140ng/mL，定量限（LOQ）分别为 0.042ng/mL 和 0.140ng/mL。在优化的麝香草酚和香芹酚条件下，建议的 MMIP 吸附剂的吸附容量分别为 64.1 和 72.6mg/g。此外，对于三次测量，线性动态范围（LDR）为 0.40-5000ng/mL，方法的准确度（RSD%）为 6.26%。通过 VSM 获得 MMIP 的饱和磁化强度为 19.0emu/g，允许快速分离吸附剂。吸附实验证实了 MMIP 对麝香草酚和香芹酚具有较大的吸附能力以及均一的结合位点。在所有加标量（20、100、200 和 500ng/mL）下，麝香草酚和香芹酚的萃取回收率分别为 96.9-103.8%和 96.6-105.4%。使用 MMIP 进行的七次解吸-再生循环的结果表明，吸附剂具有较高的稳定性。MMIP 对麝香草酚和香芹酚的吸附表现出特殊的行为，表明该方法具有选择性、简单、有效和灵活的特点。
