Résumé
This study aimed at identifying pig-hide gelatin from tortoise shell glue using ultra-performance liquid chromatography-electrospray-time of flight mass spectrometry(UPLC-ESI-QTOF-MS/MS).The samples of tortoise shell glue were digested by trypsin before the analysis on UPLC coupled with QTOF mass spectrometry.The ions at m/z 925.4 were selected as the marker peptides of pig-hide gelatin.It was found that the test results of the ions at m/z 925.4 were positive in the samples with low contents of the marker peptides of tortoise shell glue,indicating the existence of pig-hide gelatin.However,the result of bovine-hide gelatinordonkey-hide gelatin was negative,while negative results were detected in tortoiseglue standard.The finding was in conformity with previous references over the fragmentation regularity of MS/MS.In conclusion,the method can be adopted to identifying the pig-hide gelatin from tortoise shell glue and applied to the quality control of tortoise shell glue with high specificity and sensibility.
Résumé
This study aimed at developing an ultra-performance liquid chromatography electrospray time of flight-mass spectrometry (UPLC-ESI-QTOF-MS) method for the identification of bovine hide gelatine from the shell glue of the red-eared slider.Tortoise shell glue was made from the shell of red-eared slider or Reeves' turtle (Chinemys reevesii).The samples were analyzed on UPLC-ESI-QTOF-MS after being digested by trypsin,and the ions at m/z 604.8,m/z 641.3,m/z 790.8 of the marker peptides of bovine hide gelatin were detected.As a result,it was found that the test results of the ions made from the shell of red-eared slider at m/z 641.3 were positive,taking the same fragmentation regularity of MS/MS as the standard of bovine-hide gelatine,while negative results were detected from the ions made from the shell of Reeves' turtle.In conclusion,the method was simple and accurate provided a basis for distinguishing the tortoise shell glue from bovine hide,which could be also used for the quality control of tortoise shell glue.
Résumé
OBJECTIVE: To establish an analysis method for identification of gelatine ingredients in Chinese patent medicines. METHODS: Trypsin was used for hydrolysis of gelatins. The characteristic getalins analyses were identified by rapid resolution liquid chromatography (RRLC) coupled to triple quadruple mass spectrometry (QQQ-MS). Trypsin was used for hydrolysis of gelatins. RESULTS: The established present method was specific, precise and reliable. Gelatine ingredients as prescribed wereas detected for several samples. However, instead of gelatin ingredients as prescribed, unprescribed gelatine ingredients were as detected for some samples. CONCLUSION: The methodology validation is performed and the results are satisfied. The method can be used for identification of donkey-hide gelatin, oxhide gelatin, deer-horn glue and tortoise-shell glue in Chinese patent medicines, and provides a scientific reference for the study of quality control method of gelatin ingredients in Chinese Patent Medicines.