从非抗凝猪血中制备原卟啉钠方法的建立及优化研究

目的:建立并优化从非抗凝猪血中制备原卟啉钠的方法。方法:先以非抗凝猪血制得血红素,再加入硫化亚铁等经酯化、皂化反应制得原卟啉钠;采用紫外吸收光谱与红外光谱对其进行定性检测、紫外分光光度法对其进行定量检测;通过正交试验对原卟啉钠的制备方法进行优化,确定最佳工艺参数。结果:建立了从非抗凝猪血中制备原卟啉钠的方法,每千克非抗凝猪血可以制得10.6g血红素,每5g血红素可以制得3.46g原卟啉钠,所得原卟啉钠经紫外和红外光谱鉴定证实,纯度为88.8%;最佳制备工艺是酯化时甲醇-氯仿加入量为70mL∶120mL、皂化时甲苯-1mo·lL-1氢氧化钠甲醇溶液用量为50mL∶80mL、90℃加热回流2.0h。结论:所建立的制备原卟啉钠的方法操作简便,原料易得,周期短,成本低,产量较高,是一种较理想的制备原卟啉钠的方法。

Study on Establishment and Optimization of Preparation Method of Protoporphyrin Disodium from Non- anticoagulant Porcine Blood

OBJECTIVE： To establish and optimize the preparation method of protoporphyrin disodium （NAPP） from non-anticoagulant porcine blood.METHODS： Heme was prepared from non-anticoagulant porcine blood firstly.Ferrous sulfide was added into heme to prepare NAPP by saponification and esterification reaction.UV absorption spectrum and infrared spectrum were applied for qualitative test,and ultraviolet spectrophotometry was adopted for quantitative detection of NAPP.Orthogonal experiment was used to optimize the preparation method of NAPP and to determine the optimal parameters of the preparation process.RESULTS： The preparation method of NAPP from non-anticoagulant porcine blood was established.10.6 g heme could be obtained from per kilogram of non-anticoagulant porcine blood and 3.46 g NAPP could be obtained from per 5 g heme.The purity quotient of NAPP was 88.8%.The optimal parameters for the preparation of NAPP were as followed： incremental amount of methanol vs.chloroform was 70 mL ∶ 120 mL in estrification process;Incremental amount of toluene vs.1 mol·L-1 sodium hydroxide-methanol solution was 50 mL ∶ 80 mL in saponification process.The sample was extracted by continuous therma reflux at 90 ℃ for 2.0 h.CONCLUSION： The established preparation method of NAPP from non-anticoagulant porcine blood is an ideal approach for the preparation of NAPP with simple operation,abundant raw material,short preparation cycle,low cost and high yield.