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 C18色谱柱(50 mm×2.1 mm,1.8 μm),以0.1%甲酸水溶液-甲醇为流动相,梯度洗脱,流速0.3 mL·min-1,柱温40 ℃,进样量5 μL;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·mL-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·mL-1和0.16 ng·mL-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0.615~30.36 μg·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 C18 column (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·min-1, 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·mL-1 (r=0.999 7). The detection limit and quantitative limit were 0.05 ng·mL-1 and 0.16 ng·mL-1. The recovery rates were 96.0%-103.5%. Among the 90 batches of samples, 64 batches of 2,4-diaminotoluene were 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.
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