药用复合膜中2,4-二氨基甲苯的检测  

Detection of 2,4-diaminotoluene in medicinal composite membranes

作　　者：李莎 武静文 吴红洋 韩海燕 张璞 詹宇杰 雷智棋 范能全 LI Sha;WU Jing-wen;WU Hong-yang;HAN Hai-yan;ZHANG Pu;ZHAN Yu-jie;LEI Zhi-qi;FAN Neng-quan(Chonging Institute for Food and Drug Control,Chongging 401121,China;Chonging Municipal Drug Administration,Chongqing 40000,China)

机构地区：[1]重庆市食品药品检验检测研究院,重庆401121 [2]重庆市药品监督管理局检查一局,重庆400000

出　　处：《药物分析杂志》2022年第7期1234-1240,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：重庆市科研机构绩效激励引导专项项目(cstc 2019 j x j l130040)。

摘　　要：目的:建立药用复合膜中2,4-二氨基甲苯的HPLC-MS检测方法,对市场上不同厂家、不同材质的药用复合膜材料进行检测。方法:样品剪碎,用水浸泡经灭菌后过膜上机。色谱-质谱条件:采用Agilent ZORBAX Eclipse Plus C色谱柱(50 mm×2.1 mm, 1.8μm),以0.1%甲酸水溶液-甲醇为流动相,梯度洗脱,流速0.3 mL·m^(-2)in,柱温40℃,进样量5μL;离子源为电喷雾离子源(ESI),正离子模式,加热温度500℃,DP电压80 V。结果:2,4-二氨基甲苯进样浓度在0.16~52.54 ng·m^(-2)L^(-1)呈良好的线性关系(r=0.999 7),检测限和定量限分别为0.05 ng·m^(-2)L^(-1)和0.16 ng·m^(-2)L^(-1),加标回收率在96.0%~103.5%。90批次样品中检测出2,4-二氨基甲苯的样品有64批次,占71.1%,结果为0.615~30.36μg·m^(-2)。结论:该方法降低了方法检测限,简化了样品的前处理过程,操作简单,结果准确,灵敏度高,重现性好,可作为测定药用复合膜中2,4-二氨基甲苯含量的分析方法,为我国药包材标准暂未引入2,4-二氨基甲苯的检测提供方法参考和限度值设定。Objective: To establish an HPLC-MS method for the detection of 2,4-diaminotoluene in medicinal composite membranes, and test the medicinal composite membranes of different manufacturers and materials on the market. Methods: The samples were cut into pieces, soaked in water, sterilized and loaded on the machine subsequent to the filter using membrane. The chromatography-mass spectrometry condition was as follows: Agilent ZORBAX Eclipse Plus Ccolumn(2.1 mm×50 mm, 1.8 μm) was adopted, the mobile phase consisted of 0.1% formic acidaqueous solution-methanol with gradient elution at the flow rate of 0.3 mL·m^(-2)in, the column temperature was 40 ℃, the injection volume was 5 μL, the ion source was electrospray ion source(ESI), positive ion mode, the fast heating temperature was 500 ℃, the DP voltage was 80 V. Results: The injection concentration of 2,4-diaminotoluene had a good linear relationship in the range of 0.16-52.54 ng·m^(-2)L^(-1)(r=0.999 7). The detection limit and quantitative limit were 0.05 ng·m^(-2)L^(-1)and 0.16 ng·m^(-2)L^(-1). The recovery rates were 96.0%-103.5%. Among the 90 batches of samples, 64 batches of 2,4-diaminotoluenewere detected, accounting for 71.1%, and the results were 0.615-30.36 μg·m^(-2). Conclusion: This method reduces the detection limit of the method, simplifies the pretreatment process of the sample, and has the advantages of simple ope-ration, accurate results, high sensitivity and good reproducibility, as an analytical method for detection of 2,4-diaminotoluene in medicinal composite membranes. It can provide a reference for testing methods and limit value setting for the detection of 2,4-diaminotoluene that has not yet been introduced into drug packaging material standards in China.

关 键 词：液相色谱-质谱法 药用复合膜 2 4-二氨基甲苯 含量分析 限度值 

分 类 号：R917[医药卫生—药物分析学]