Quantitative determination of residual 1,4-dioxane in 3D printed bone scaffold

	Quantitative determination of residual 1,4-dioxane in 3D printed bone scaffold
	Ling Li; Jing Long; Huijuan Cao; Long Li; Tingting Tang; Xinghua Xi; Ling Qin; Yuxiao Lai
刊名	Journal OF Orthopaedic Translation
	2017
文献子类	期刊论文
英文摘要	Background/Objective A novel porous scaffold poly (lactide-co-glycolide) and tricalcium phosphate (PLGA/TCP) was developed by 3D printing technology for bone defect repair. As a class 2 solvent with less severe toxicity, content of residual 1, 4-dioxane1,4-dioxane in this newly developed scaffolds should be rigorously controlled. To date, established methods for 1,4-dioxane have been used for quantification analysis in liquid or liquid-like samples, such as drinking water, waste water, vaccine and cosmetics. But there was no method to be used for quantification analysis in solid samples, like scaffolds, the pre-treatment is a necessary step to select a proper solvent before analysis . A specificity, precise and accuracy In this study, a headspace, gas chromatography-mass spectrometric (HS-GC-MS) method and related testing protocol were developed for quantitative determination of 1, 4-dioxane1,4-dioxane in the translation process of PLGA/TCP composite scaffolds. Methods Matrix effect analysis was used to optimize the pretreatment method of the scaffolds. Then the procedure for testing 1,4-dioxane using HS-GC-MS was set up. The accuracy, precision and robustness of this newly developed quantitative method were also validated before quantification of 1,4-dioxane in the scaffolds with different drying procedures. Results Compared to Na2CO3 solutiondimethyl formamide (DMF), using dimethyl formamide (DMF) Na2CO3 solution to exact the scaffold got highproper sensitivity to satisfy the detection. In the meantime, butthere is no serious matrix effects to interrupt. So the optimized procedure was determined as: the scaffolds were dissolved in DMF and kept at 8090 ℃ for 40 minutes, then subjected to HP-5MS column, and detected by mass spectrum. Recovery experiments gave 97.9%-100.7% recovery for 1, 4- dioxane. The linear range for 1, 4-dioxane1,4-dioxane was determined as 1-40 ppm with liner correlation coefficient ≥ 0.9999. Intra-day and inter-day precision was determined that showed a within relative standard deviation (RSD) of below 0.68%. The passable drying procedure was related to lyophilizing the scaffolds for 2 days and drying in vacuum for 7 days. Conclusion This is the first quantitative method established to test 1,4-dixoane in a novel scaffold. This method was validated with good accuracy and reproducibility, and met the methodological requirements of the Guideline 9101 documented in the Chinese Pharmacopoeia 2015 Edition. Then, the method was applied as an enterprise standard to optimize the drying process of scaffolds and monitor the quality of scaffolds in the industrialization process. It is an important file in medical device approval and registration. The Translational Potential This quantitative method is a key technical method in the translation of scaffolds. The porous scaffold will be translated as a medical devices to implant the bone defect site. Safe is the one important charater. 1,4-dioxane as a class 2 solvent with less severe toxicity is the main solvent in the fabrication of PLGA/TCP scaffolds. The content of residual 1,4-dioxane in this newly developed scaffolds will treat to the safety of scaffolds. It is necessary to be rigorously controlled. But there is no method to be used for content detection of scaffolds so far. This is the first quantitative method established to test 1,4-dixoane in a novel scaffold. It will be used for monitoring the content of 1,4-dioxane in the translation to improve the manufacturing technique in order to decrease the content of 1,4-dioxane to the limit of government standard. Also will be used for controlling scaffolds quality as a daily detection to comply with safety requirements.
语种	英语
内容类型	期刊论文
源URL	[http://ir.siat.ac.cn:8080/handle/172644/12149]
专题	深圳先进技术研究院_医工所
作者单位	Journal OF Orthopaedic Translation
推荐引用方式 GB/T 7714	Ling Li,Jing Long,Huijuan Cao,et al. Quantitative determination of residual 1,4-dioxane in 3D printed bone scaffold[J]. Journal OF Orthopaedic Translation,2017.
APA	Ling Li.,Jing Long.,Huijuan Cao.,Long Li.,Tingting Tang.,...&Yuxiao Lai.(2017).Quantitative determination of residual 1,4-dioxane in 3D printed bone scaffold.Journal OF Orthopaedic Translation.
MLA	Ling Li,et al."Quantitative determination of residual 1,4-dioxane in 3D printed bone scaffold".Journal OF Orthopaedic Translation (2017).