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1.
Article in Chinese | WPRIM | ID: wpr-923495

ABSTRACT

@#Due to the complex components of polysorbate 80, analysis is time-consuming and labor-intensive, so there is an urgent need to find a method for rapid analysis of polysorbate 80 components.In this study, 10 batches of samples collected from 3 domestic and foreign enterprises were analyzed by UHPLC-HRMS, with the being further results were analyzed by the ExcipientProfiler software and supplemented by the extended database.The results showed that the ExcipientProfiler software could quickly identify the [M+Na]+ peak in the mass spectrogram, and obtain the information of component distribution, the numbers of components and the degree of polymerization of the sample.Meanwhile, the numbers of components obtained by the ExcipientProfiler software could be used to distinguish the injection grade samples from the ordinary grade samples by systematic clustering analysis.In addition, it was found through further supplement that the sample contained other fatty acid ester components by manually searching the relevant extended database.The polyoxyethylene sorbitan tetraoleate components were found in the sample according to the analysis of mass spectrum data.Therefore, although this method is fast and simple, it is necessary to add polyoxyethylene sorbitan tetraoleate components and other fatty acid ester components to further supplement the information in the ExcipientProfiler software, so that it can be better used for the analysis of polysorbate 80.

2.
Article in Chinese | WPRIM | ID: wpr-804550

ABSTRACT

@#A novel method was developed for the content assay and related substances determination of neomycin sulfate by high performance liquid chromatography combined with pulsed amperometric detection(HPLC-PAD). The HPLC was performed on Thermo AcclaimTMAmG C18(4. 6 mm×150 mm, 3 μm). The mobile phase consisted of aqueous solution with 2% trifluoroacetic acid containing 0. 01% pentafluoropropionic acid and 0. 6%NaOH. The pulsed amperometric detector was operated with aquadruple-potential waveform for the detection. Neomycin B, Neomycin C and thirteen related substances were adequately separated by the established HPLC conditions. The limits of detection(LOD)and quantification(LOQ)of neomycin B and neomycin C were both 1. 75 ng and 3. 5 ng, respectively. Good linearities of neomycin B and neomycin C were found in their respective ranges which their correlation coefficients were greater than 0. 998 5. The established method is characterized by high specificity, sensitivity and wide range of linearity which has a good application prospect and provides the basis for improving the standard and quality control of neomycin sulfate.

3.
Article in Chinese | WPRIM | ID: wpr-811775

ABSTRACT

@#To establish a RP-HPLC method for the determination of content of sisomicin sulfate and sodium chloride injection. Thermo Aminoglycoside RP 18(4. 6 mm ×150 mm, 3 μm)column was used. The mobile phase consisted of Sodium heptane sulfonate solution(take 6 g of sodium heptane sulfonate, add 0. 1 mol/L potassium dihydrogen phosphate solution and dilute to 1 000 mL, adjust the pH to 1. 5 with phosphoric acid)- acetonitrile(77∶23). The detection wavelength was 205 nm, the flow rate was 1. 0 mL/min. and the column temperature was 35 °C. The separation of sisomicin peaks with related substances and the degradation products was good. The linear range of the peak area with sisomicin was 0. 010 024-1. 002 4 mg/mL(Y=4. 210 2×106 X+9. 107 0×103, r=0. 999 9, n=7), the detection limit was 0. 6 ng, the limit of quantification was 2 ng, and the recovery rate was at 99. 1%-100. 9%(RSD< 1. 0%, n=9). The method is sensitive, exclusive, accurate and suitable for the determination of sisomicin. Compared with the antibiotic microbiological test method, the specificity is better, the confidence interval of the result is narrowed, and the test time is saved.

4.
Article in Chinese | WPRIM | ID: wpr-811763

ABSTRACT

@#This study was to evaluate quality consistency of domestic generic and reference preparations. Content and related substances of domestic generic preparations and reference preparation were inspected according to Chinese Pharmacopeia 2015. Then the basic solution for determining dissolution curve was established through preliminary experiment and validation for determination. The dissolution curves of domestic rifampicin capsules and reference preparation were compared in four dissolution mediums: HCl(pH 1. 2), PBS(pH 4. 0), PBS(pH 6. 8)and pure water, respectively. Results showed that the content and related substances of domestic generic and reference preparations complied with the quality standard, but impurity profile displayed that impurities in domestic generic preparations were less than those in the reference preparation, with the content of rifampin quinine being especially less. Furthermore, dissolution of domestic generic and reference preparations were compared, and their dissolution curves were not similar. It is suggested that consistency between domestic rifampicin capsules and reference preparation should be evaluated by bioequivalence test.

5.
Article in Chinese | WPRIM | ID: wpr-617553

ABSTRACT

An RP-HPLC method was established to separate the related substances of benzyl hydroxybenzoate.The separation was carried out on a Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column.The mobile phase was methonal-0.1% glacial acetic acid,using linear gradient elution,and the detection wavelength was 254 nm.There was a good linear relationship between 0.051-101.88 μg/mL (r =1.00) and 0.050-99.48 μg/mL(r =0.999 8) for benzyl hydroxybenzoate and p-hydroxybenzoic acid,repectively.The average recovery of p-hydroxybenzoic acid was 100.3% and the RSD was 0.95%.The LOQ of p-hydroxybenzoic acid was 0.24 ng.The detected impurities were also identified by UPLC-Q-TOF.The established method is accurate and reproducible,and could be used for the quality control of benzyl hydroxybenzoate.

6.
Article in Chinese | WPRIM | ID: wpr-811846

ABSTRACT

@#This study aimed to isolate and prepare highly purified impurity C from doxycycline hyclate by a preparative HPLC method and to inspect the toxicity and in vitro antimicrobial activity of the impurity C of doxycycline hyclate. The solution of doxycycline hyclate treated with heat produced a solution containing 10% of impurity C which was firstly separated by the Sapphire C18(21. 2 mm×250 mm, 5 μm)column with 0. 1% acetic acid-acetonitrile(83 ∶17)as the mobile phase at 20 mL/min. Secondly, rotary evaporation of the eluted solution at the time of 8. 4 min was performed at 50 °C to remove organic solvent. Then the target product was prepared after freeze drying of evaporated solution adjusting pH to 1. 8 with formic acid. The target product was identified with ultraviolet absorbance(UV), infrared(IR), mass spectrometry(MS)and nuclear magnetic resonance(NMR), and its purity was be determined by HPLC. Meanwhile, cytotoxicity and genotoxicity in the Chinese hamster lung cells, toxicity on the development of zebrafish embryos and in vitro antimicrobial activity were compared among impurity C of doxycycline hyclate, doxycycline, metacycline and β-doxycycline. Results showed that prepared product was confirmed to be the impurity C of doxycycline hyclate. Its purity was 90. 1%, which had been the highest so far. In the cellular toxic tests and genetic toxic tests of Chinese hamster lung cells, impurity C of doxycycline hyclate, doxycycline, metacycline and β-doxycycline were somewhat toxic to Chinese hamster lung cells. Toxicity gradually decreased from doxycycline, impurity C of doxycycline hyclate, β-doxycycline to metacycline from -S9mix test results; toxicity gradually decreased from doxycycline, β-doxycycline, impurity C of doxycycline hyclate to metacycline from +S9mix test results; the aberration rate of all the tested related substances was less than 5%, and no obvious genotoxicity was found. According to test results of the development of zebrafish embryos, impurity C of doxycycline hyclate showed the strongest teratogenicity and lethality. Invitro antimicrobial tests revealed that impurity C of doxycycline hyclate had a weaker antimicrobial activity, and invitro antimicrobial activity potential of the tested compounds followed the order: metacycline, doxycycline, impurity C of doxycycline hyclate, β-doxycycline. Studies on safety and effectiveness indicated that impurity C of doxycycline hyclate belonged to toxic and ineffective impurity and need to be controlled individually in quality standard. A useful suggestion was given to revise the quality standard of doxycycline hyclate and its preparation in the current Pharmacopoeia of the People′s Republic of China.

7.
Article in Chinese | WPRIM | ID: wpr-480329

ABSTRACT

Aim: To establish an HPLC method for the determination of secnidazole and its related substances, and to elucidate the structure of the main related substances. Methods: HPLC was performed on an Agilent C_(18) (150 mm × 4. 6 mm, 5 μm) column. The mobile phase consisted of acetonitrile and 0. 1% formic acid solution( 10 : 90). The detection wavelength was set at 320 nm and the column oven was maintained at 30 ℃. The mass spec-trometry detector was equipped with an ESI source with a temperature of 350 ℃, and set at positive ion monito-ring model The spray chamber pressure was 0. 34 MPa. The drying gas flow rate was 10 L/min. Results: Sec-nidazole was completely separated from the impurities. The calibration curve of secnidazole was linear over the range of 0. 10-1 500. 0 μg/mL with the correlation coefficient of 0. 999 9. The contents of secnidazole in the sam-ples were 100.5%, 100.3% and 100.7%, respectively, and those of the related substances were 0.463%, 0. 488% and 0.465%, respectively. The three related substances were identified by HPLC-UV-MS~n as 2-methyl-5-nitroimida-zole and the isomerides of secnidazole, respectively. Conclusion: The developed method is reliable for the quality control and determination of related substances of secnidazole.

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