北京生物醫(yī)學(xué)工程

高效液相色譜法測(cè)定聚乳酸中乳酸單體殘留量

Determination of lactic acid monomer residues in polylactideby high performance liquid chromatography

作者：劉曦林紅賽崔永平

單位：北京市醫(yī)療器械檢驗(yàn)所(北京101111)<p></p>

關(guān)鍵詞：聚乳酸；乳酸單體；殘留量；高效液相色譜

分類號(hào)：R318.04

出版年·卷·期（頁碼）：2017·36·5（513-516）

摘要：

目的通過高效液相色譜法(high performance liquid chromatography，HPLC)測(cè)定聚乳酸材料中乳酸單體的殘留量，完善此類材料的質(zhì)量評(píng)價(jià)方法。方法用三氯甲烷溶解聚乳酸材料樣品后，加入等體積磷酸二氫鉀水溶液(20mmol/L，pH=2.87)渦旋振蕩，靜置分層后取上清液，采用C18 Synergi 4u Hydro-RP 80A 色譜柱，進(jìn)樣20μL，以流速0.6mL/min，磷酸二氫鉀水溶液為流動(dòng)相，柱溫30℃，紫外檢測(cè)波長(zhǎng)210nm，外標(biāo)法定量并進(jìn)行方法學(xué)研究，包括液相色譜系統(tǒng)適應(yīng)性、線性范圍、檢出限、定量限、回收率。結(jié)果本方法中理論塔板數(shù)為10660，拖尾因子為1.32，分離度為3.81，重復(fù)性相對(duì)標(biāo)準(zhǔn)偏差為0.54%(n=5)，乳酸在濃度1.05~105μg/mL范圍內(nèi)與峰面積保持良好的線性關(guān)系(r=0.999979)，檢出限為0.42μg/mL，定量限為1.05μg/mL，萃取平均回收率為94.76%(n=6)，其相對(duì)標(biāo)準(zhǔn)偏差為3.04%。聚乳酸樣品中乳酸單體平均殘留量為144.17μg/g。結(jié)論高效液相色譜法測(cè)定聚乳酸中乳酸單體殘留量具有良好的線性范圍，準(zhǔn)確度高，重復(fù)性好，萃取回收率較高且操作簡(jiǎn)單，可用于聚乳酸材料中乳酸單體殘留量測(cè)定。

Objective To determinate lactic acid monomer residues in polylactide by high performance liquid chromatography(HPLC)，and to perfect evaluation method of this kind of materials. Methods Polylactide was dissolved in trichloromethane，then monopotassium phosphate solution(20mmol/L，pH=2.87) was added. The mixed solution was oscillated and then kept still. Lactic acid monomer residual in the supernatant was determined by high performance liquid chromatography with C18 Synergi 4u Hydro-RP 80A column. The injection volum was 20μL; the flow rate was 0.6mL/min; the mobile phases was monopotassium phosphate solution(20mmol/L，pH=2.87); the column temperature was 30℃; the UV-light detectation wavelength was 210nm. The methodology consisted of system suitability，linearity range，detectation limit，limit of quantitation，recovery rate. Results In this method,the theoretical plate number was 10660; the tailing factor was 1.32; the resolution was 3.81; the relative standard deviation of the repeatability was 0.54%(n=5); the concentration range 1.05—105μg/mL of lactic acid kept good linear relationships with peak area and the coefficient correlations were 0.999979%; the limit of detection was 0.42μg/mL; the limit of quantitation was 1.05μg/mL; the average extraction recovery rate was 94.76%(n=6) with relative standard deviation of 3.04%. The average content of lactic acid monomer residual in the sample was 144.17μg/g. Conclusions This method is simple and has good linear relationship,high precision and repeatability,which can be applied to determinate lactic acid monomer residues in polylactide.

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