| Some of the features in the fingerprints can show the relevant information of the donors.In order to make full use of the fingerprints left in the crime scene and further characterize the fingerprints of the donors,we can obtain more data(such as diabetes)of the criminal in the fingerprints.Therefore,there is an urgent need for an efficient,rapid,stable,and accurate extraction and detection method for the Hypoglycemic in fingerprints.In this essay,sulfonylureass for the treatment of diabetes were studied.There are four drugs with higher market share as follows: Glibenclamide,Glimepiride,Glipizide and Gliclazide.Drugs were selected as the study subjects.The experimental studied on things as follows:1.A chromatographic and mass spectrometric detection method was developed for the detection of glibenclamide,glimepiride,glipizide and gliclazide;2.The extraction of sulphonylureass in fingerprints was established.The method of purification was compared and the extraction and purification effects using methanol and acetonitrile as precipitants were compared and investigated.3.The factors of objects that affect the detection of sulphonylureass in the fingerprints were studied;4.The factors of fingerprinting that affect the detection of sulphonylureass in the fingerprints were studied.The main results of the study are as follows:1.Use ACQUITY UPLC HSS C18(2.1×50 mm,1.8 μm)as the column;mobile phase organic phase is acetonitrile,aqueous phase is 0.1% aqueous formic acid,use gradient elution procedure.the MRM scan mode was used.The quantitative ion pair was 494.05 > 169.01 of glibenclamide,and the qualitative ion pair was 494.05 > 169.01,494.05 > 368.97;the quantitative ion pair of glimepiride was 491.26 > 126.14,and the qualitative ion pair was 491.26> 126.14,491.26> 352.15;the quantitative ion pair of glipizide was 324.16 > 127.12,and the qualifier ion pair was 324.16 > 127.12,324.16 > 110.12,the quantitative ion pair of gliclazil was 446.21> 103.04,and the qualitative ion pair was 446.21> 103.04,446.21> 321.16,The limit of detection of glibenclamide was 0.02 ng / mL and the limit of quantitation was 0.1 ng / mL.The limit of detection of glimepiride was 0.02 ng / mL and the limit of quantitation was 0.1 ng / mL.The limit of detection of glipizide was 0.01 ng / mL,and the limit of quantitation was 0.1 ng / mL;The limit of detection of gliclazide was 0.01 ng / mL,and the limit of quantitation was 0.05 ng / mL;this method has a good range of 1 ~ 1000 ng / mL Linear relationship,the correlation coefficient is above 0.99.2.Using the protein precipitation method process sulfonylureas hypoglycemic agents of the fingerprints.When use methanol as a precipitant its matrix effect coefficient between 0.89 to 1.16,the recovery rate between 68% and 123%,There is a good linear relationship of this method between 0.25 ng / patch(swab)to 250 ng / patch(swab),intraday precision and daytime precision RSD≤14.50%;When use acetonitrile as the precipitant its matrix effect coefficient between 0.79 and 1.48.The recovery rates ranged from 0.50 to 1.14.This method has a good linearity in the range of 0.25 ng / patch(swab)to 250 ng / patch(swab),with intraday precision and daytime precision RSD≤14.72%.3.Different objects have different retention ability for sulphonylurea hypoglycaemic agents.For common permeable objects,the retention ability of paper towels is stronger,and the retention capacity of wet wipes and cotton cloth is poorer.For common non-permeable objects.The retention ability of the tiles with rough surfaces is the strongest,and other objects with a smooth surface are not much different.4.The methods commonly used in all kinds of objects will lose the drug components of the fingerprints,but in most cases will not affect the detection of drug ingredients.Among them,ninhydrin expression method,“502 gel” smear method and magnetic brushing method showed that fingerprints had less effect on detection;sesquidione method,gold powder and silver paint showed fingerprints had a greater impact on detection. |
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