Method for detecting 2-mercaptobenzothiazole in ceftriaxone sodium
A technology of mercaptobenzothiazole and ceftriaxone sodium, which is applied in the field of detection of 2-mercaptobenzothiazole in ceftriaxone sodium, can solve problems such as uncontrollable safety of ceftriaxone sodium, and improve drug safety and sensitivity High and control the effect of product quality
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Embodiment 1
[0067] Prepare the reference substance solution: accurately weigh the 2-mercaptobenzothiazole reference substance, dissolve it in a solvent, and quantitatively dilute it into a 2-mercaptobenzothiazole solution with a concentration of 0.1 μg / mL as the reference substance solution. The solvent is water and Acetonitrile is the mixed solution obtained by mixing the ratio of 60:40 by volume;
[0068] Prepare the test solution: dissolve ceftriaxone sodium in the solvent, and quantitatively dilute it into a solution with a concentration of 10 mg / mL, as the test solution; the solvent is water and acetonitrile mixed in a ratio of 60:40 by volume to obtain the mixture;
[0069] Reference substance solution and need testing solution are carried out HPLC analysis, obtain the spectrogram of reference substance solution and need testing solution, the condition of HPLC analysis is:
[0070] Chromatographic column: Agilent ZORBAX SB-Aq C18, 4.6mm×250mm, 5μm;
[0071] Mobile phase: 1% formic...
Embodiment 2
[0078] Exclusive experiment:
[0079] Prepare a blank solvent: water and acetonitrile are mixed in a volume ratio of 60:40 to obtain a blank solvent;
[0080] Prepare test solution and reference substance solution according to the method of embodiment 1;
[0081] Blank solvent, reference substance solution, need testing solution are carried out high performance liquid chromatography analysis according to the condition in embodiment 1 successively, the result is as follows Figure 1~4 and shown in Table 1.
[0082] Depend on Figure 1~4 As can be seen from Table 1, the blank solvent does not interfere with the determination of the sample, and in the test solution, the degree of separation between 2-mercaptobenzothiazole and adjacent peaks is greater than 1.5, indicating that the specificity of the detection method provided by the present invention is good.
[0083] The spectrogram information of table 1 blank solvent, reference substance solution and need testing solution
...
Embodiment 3
[0087] Determination of quantitation limit and detection limit:
[0088] The reference substance solution was diluted step by step, and carried out high performance liquid chromatography analysis according to the aforementioned test method, the concentration at which the signal-to-noise ratio (S / N) was about 10 was used as the limit of quantitation concentration, and the concentration when the S / N was about 3 was used as Detection limit concentration, the results are shown in Table 3, as Figure 5 and Figure 6 Shown are the HPLC chromatograms of the solutions with the quantification limit concentration and detection limit concentration respectively. As can be seen from Table 3, the quantification limit concentration is equivalent to the percentage (%) of sample concentration (10mg / mL) and is 0.00005% (i.e. 0.5ppm), and the detection limit concentration is equivalent to the percentage (%) of sample concentration of 0.000015% (i.e. 0.15ppm ), indicating that the detection met...
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