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.
LI Sha, WU Jing-wen, WU Hong-yang, HAN Hai-yan, ZHANG Pu, ZHAN Yu-jie, LEI Zhi-qi, FAN Neng-quan
. Detection of 2,4-diaminotoluene in medicinal composite membranes*[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(7)
: 1234
-1240
.
DOI: 10.16155/j.0254-1793.2022.07.17
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