Sude Oflu , Sezin Erarpat , Buse Tuğba Zaman , Ömer Tahir Günkara , Sezgin Bakırdere , Fatma Turak
{"title":"四极杆同位素稀释质谱-同时衍生化-喷雾辅助液滴形成-液相微萃取联合气相色谱质谱法测定人尿和血清样品中的甲基苯丙胺","authors":"Sude Oflu , Sezin Erarpat , Buse Tuğba Zaman , Ömer Tahir Günkara , Sezgin Bakırdere , Fatma Turak","doi":"10.1016/j.vascn.2022.107207","DOIUrl":null,"url":null,"abstract":"<div><p>In this study, an analytical method with high accuracy and precision was developed for the determination of methamphetamine in human urine and serum samples by gas chromatography–mass spectrometry (GC–MS). A simultaneous derivatization and spray assisted droplet formation-liquid phase microextraction (SADF-LPME) method was proposed to derivatize and preconcentrate target analyte. Quadruple isotope dilution (ID<sup>4</sup>) was used to provide high accuracy and precision for methamphetamine determination in the samples. After the optimization studies for the derivatization and microextraction parameters, limit of detection (LOD) and limit of quantitation (LOQ) for the developed SADF-LPME method were found to be 48.0 and 159.9 μg/kg, respectively. Recovery studies were implemented to verify the applicability and accuracy of the developed method for human urine and serum samples. The SADF-LPME method gave low percent recovery results (30.5–61.0%) for the spiked urine and serum samples showing that it failed to minimize or eliminate matrix effects for the analyte. Hence, methamphetamine acetamide-<em>d3</em> was synthesized and purified in our research laboratory to be used as methamphetamine isotopic analogue in the ID<sup>4</sup> method. When the SADF-LPME method was combined with ID<sup>4</sup>, the percent recovery values for urine and serum samples were calculated as 99.7–100.0% and 99.4–100.2%, respectively. These results demonstrated the applicability and accuracy of the proposed method for urine and serum samples.</p></div>","PeriodicalId":16767,"journal":{"name":"Journal of pharmacological and toxicological methods","volume":null,"pages":null},"PeriodicalIF":1.3000,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"5","resultStr":"{\"title\":\"Combination of quadrupole isotope dilution mass spectrometry with simultaneous derivatization and spray assisted droplet formation-liquid phase microextraction for the determination of methamphetamine in human urine and serum samples by gas chromatography mass spectrometry\",\"authors\":\"Sude Oflu , Sezin Erarpat , Buse Tuğba Zaman , Ömer Tahir Günkara , Sezgin Bakırdere , Fatma Turak\",\"doi\":\"10.1016/j.vascn.2022.107207\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>In this study, an analytical method with high accuracy and precision was developed for the determination of methamphetamine in human urine and serum samples by gas chromatography–mass spectrometry (GC–MS). A simultaneous derivatization and spray assisted droplet formation-liquid phase microextraction (SADF-LPME) method was proposed to derivatize and preconcentrate target analyte. Quadruple isotope dilution (ID<sup>4</sup>) was used to provide high accuracy and precision for methamphetamine determination in the samples. After the optimization studies for the derivatization and microextraction parameters, limit of detection (LOD) and limit of quantitation (LOQ) for the developed SADF-LPME method were found to be 48.0 and 159.9 μg/kg, respectively. Recovery studies were implemented to verify the applicability and accuracy of the developed method for human urine and serum samples. The SADF-LPME method gave low percent recovery results (30.5–61.0%) for the spiked urine and serum samples showing that it failed to minimize or eliminate matrix effects for the analyte. Hence, methamphetamine acetamide-<em>d3</em> was synthesized and purified in our research laboratory to be used as methamphetamine isotopic analogue in the ID<sup>4</sup> method. When the SADF-LPME method was combined with ID<sup>4</sup>, the percent recovery values for urine and serum samples were calculated as 99.7–100.0% and 99.4–100.2%, respectively. These results demonstrated the applicability and accuracy of the proposed method for urine and serum samples.</p></div>\",\"PeriodicalId\":16767,\"journal\":{\"name\":\"Journal of pharmacological and toxicological methods\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":1.3000,\"publicationDate\":\"2023-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"5\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of pharmacological and toxicological methods\",\"FirstCategoryId\":\"3\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S1056871922000545\",\"RegionNum\":4,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"PHARMACOLOGY & PHARMACY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of pharmacological and toxicological methods","FirstCategoryId":"3","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S1056871922000545","RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"PHARMACOLOGY & PHARMACY","Score":null,"Total":0}
Combination of quadrupole isotope dilution mass spectrometry with simultaneous derivatization and spray assisted droplet formation-liquid phase microextraction for the determination of methamphetamine in human urine and serum samples by gas chromatography mass spectrometry
In this study, an analytical method with high accuracy and precision was developed for the determination of methamphetamine in human urine and serum samples by gas chromatography–mass spectrometry (GC–MS). A simultaneous derivatization and spray assisted droplet formation-liquid phase microextraction (SADF-LPME) method was proposed to derivatize and preconcentrate target analyte. Quadruple isotope dilution (ID4) was used to provide high accuracy and precision for methamphetamine determination in the samples. After the optimization studies for the derivatization and microextraction parameters, limit of detection (LOD) and limit of quantitation (LOQ) for the developed SADF-LPME method were found to be 48.0 and 159.9 μg/kg, respectively. Recovery studies were implemented to verify the applicability and accuracy of the developed method for human urine and serum samples. The SADF-LPME method gave low percent recovery results (30.5–61.0%) for the spiked urine and serum samples showing that it failed to minimize or eliminate matrix effects for the analyte. Hence, methamphetamine acetamide-d3 was synthesized and purified in our research laboratory to be used as methamphetamine isotopic analogue in the ID4 method. When the SADF-LPME method was combined with ID4, the percent recovery values for urine and serum samples were calculated as 99.7–100.0% and 99.4–100.2%, respectively. These results demonstrated the applicability and accuracy of the proposed method for urine and serum samples.
期刊介绍:
Journal of Pharmacological and Toxicological Methods publishes original articles on current methods of investigation used in pharmacology and toxicology. Pharmacology and toxicology are defined in the broadest sense, referring to actions of drugs and chemicals on all living systems. With its international editorial board and noted contributors, Journal of Pharmacological and Toxicological Methods is the leading journal devoted exclusively to experimental procedures used by pharmacologists and toxicologists.