Method for detecting the content of genotoxic impurity benzyl bromide in drug
A detection method and genotoxicity technology, which is applied in the field of detection of genotoxic impurity benzyl bromide content in drugs, can solve problems such as the blank detection method of benzyl bromide, and achieve the effects of reliable detection, strong specificity, and simple sample processing
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Embodiment 1
[0027] Embodiment 1: test preparation
[0028] 1. Instrument and reagent preparation
[0029] instrument:
[0030] Shimadzu LC-20AT high performance liquid chromatograph (including binary high pressure pump, column thermostat, autosampler, UV detector, LabSolutions chromatographic workstation, Japan Shimadzu); Sartorius SQP analytical balance (Beijing Sartorius Scientific Instruments Ltd).
[0031] Reagent:
[0032] Both methanol and acetonitrile were produced by Tiandi Company (chromatographically pure); dimethyl sulfoxide (Shanghai Aladdin Biochemical Technology Co., Ltd., chromatographically pure); benzyl bromide (Shanghai Macklin Biochemical Technology Co., Ltd., chromatographically pure); The water used is Wahaha purified water.
[0033] 2. Solution preparation
[0034] (1) Benzyl bromide reference substance solution: Accurately weigh an appropriate amount of benzyl bromide reference substance, put it in a measuring bottle, and quantitatively dilute it with acetonitr...
Embodiment 2
[0044] Embodiment 2: specificity test
[0045] Take 20 μl each of the blank solvent, the reference substance solution, the test solution and the standard-added test solution, and inject them into the liquid chromatograph respectively, and record the chromatogram. The results are shown in Figure 1 to Figure 4 . The result shows that the matrix in the blank solvent and the test sample does not interfere with the determination of benzyl bromide, and the degree of separation between benzyl bromide and adjacent chromatographic peaks is greater than 1.5, showing that the specificity of the method of the present invention is good.
Embodiment 3
[0046] Embodiment 3: system suitability test
[0047] Accurately weigh 25mg of the drug, put it in a 5ml volumetric flask, add 0.6ml of dimethyl sulfoxide, shake to dissolve, then precisely add an appropriate amount of benzyl bromide reference substance, put it in the same volumetric flask, and dilute quantitatively with acetonitrile to prepare each 1ml contains 5mg of drug and 150ng of benzyl bromide mixed solution. Under the chromatographic conditions as in Example 1, samples were injected continuously for 6 times, the chromatogram was recorded, and the retention time of benzyl bromide, the peak area, and the RSD value of the resolution of adjacent chromatographic peaks were calculated. The results are shown in Table 1 below.
[0048] Table 1 Results of system suitability test
[0049]
[0050] The results in Table 1 show that the RSD of the retention time of benzyl bromide is 0.12%, and the RSD of the peak area is 8.06%, which meets the requirements.
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