跳轉至內容
Merck
  • Capillary electrophoresis-mass spectrometry determination of morphine and its isobaric glucuronide metabolites.

Capillary electrophoresis-mass spectrometry determination of morphine and its isobaric glucuronide metabolites.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2015-01-16)
Theresa A Isbell, Erin C Strickland, Jennifer Hitchcock, Gregory McIntire, Christa L Colyer
摘要

The determination of morphine and its isobaric metabolites morphine-3-beta-d-glucuronide (M3G) and morphine-6-beta-d-glucuronide (M6G) is useful for therapeutic drug monitoring and forensic identification of drug use. In particular, capillary electrophoresis with mass spectrometry (CE-MS) represents an attractive tool for opioid analysis. Whereas volatile background electrolytes in CE often improve electrospray ionization for coupled MS detection, such electrolytes may reduce CE separation efficiency and resolution. To better understand the effects of background electrolyte (BGE) composition on separation efficiency and detection sensitivity, this work compares and contrasts method development for both volatile (ammonium formate and acetate) and nonvolatile (ammonium phosphate and borate) buffers. Peak efficiencies and migration times for morphine and morphine metabolites were optimal with a 25mM ammonium borate buffer (pH=9.5) although greater sensitivities were achieved in the ammonium formate buffer. Optimized CE methods allowed for the resolution of the isobaric morphine metabolites prior to high mass accuracy, electrospray ionization quadrupole time-of-flight (ESI-QTOF) MS detection applicable to the analysis of urine samples in under seven minutes. Urine sample preparation required only a 10-fold dilution with BGE prior to analysis. Limits of detection (LOD) in normal human urine were found to be 1.0μg/mL for morphine and 2.5μg/mL for each of M3G and M6G by CE-ESI-QTOF-MS. These LODs were comparable to those for CE-UV analysis of opioid standards in buffer, whereas CE-ESI-QTOF-MS analysis of opioid standards in buffer yielded LODs an order of magnitude lower. Patient urine samples (N=12) were analyzed by this new CE-ESI-QTOF-MS method and no significant difference in total morphine content relative to prior liquid chromatography-mass spectrometry (LC-MS) results was found as per a paired-t test at the 99% confidence level. Whereas the LC-MS method applied to these samples determined only total morphine content, this new CE-ESI-QTOF-MS method allowed for species differentiation in addition to total morphine determination. By this method, it was found that M3G and M6G metabolites were present in a 5:1 concentration ratio, on average, in patient samples. Therefore, the CE-ESI-QTOF-MS method not only allows for total morphine concentration determination comparable to established LC-MS methods, but also allows for differentiation between morphine and its trace glucuronides, yielding additional biochemical information about drug metabolism.

材料
產品編號
品牌
產品描述

Sigma-Aldrich
氢氧化铵 溶液, ACS reagent, 28.0-30.0% NH3 basis
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸, glacial, ACS reagent, ≥99.7%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸, glacial, ReagentPlus®, ≥99%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
甲酸, reagent grade, ≥95%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, ACS reagent, ≥85 wt. % in H2O
暫時無法取得訂價和供貨情況
Sigma-Aldrich
硼酸, ACS reagent, ≥99.5%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
甲酸, ACS reagent, ≥96%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
氢氧化铵 溶液, 28% NH3 in H2O, ≥99.99% trace metals basis
暫時無法取得訂價和供貨情況
Sigma-Aldrich
甲酸, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, 85 wt. % in H2O, 99.99% trace metals basis
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, ACS reagent, ≥85 wt. % in H2O
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸, glacial, ≥99.99% trace metals basis
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸 溶液, suitable for HPLC
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥85%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
氢氧化铵 溶液, puriss., 30-33% NH3 in H2O
暫時無法取得訂價和供貨情況
Sigma-Aldrich
硼酸, ReagentPlus®, ≥99.5%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, crystalline, ≥99.999% trace metals basis
暫時無法取得訂價和供貨情況
Sigma-Aldrich
甲酸, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
硼酸, BioReagent, for molecular biology, suitable for cell culture, suitable for plant cell culture, ≥99.5%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, puriss. p.a., crystallized, ≥99.0% (T)
暫時無法取得訂價和供貨情況
Sigma-Aldrich
甲酸, ACS reagent, ≥88%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
硼酸, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., buffer substance, ≥99.8%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
氢氧化铵 溶液, puriss. p.a., reag. ISO, reag. Ph. Eur., ~25% NH3 basis
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, puriss., meets analytical specification of Ph. Eur., BP, NF, FCC, 85.0-88.0%
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸 溶液, 85 wt. % in H2O, FCC, FG
暫時無法取得訂價和供貨情況
Sigma-Aldrich
乙酸, for luminescence, BioUltra, ≥99.5% (GC)
暫時無法取得訂價和供貨情況
Sigma-Aldrich
磷酸, BioUltra, ≥85% (T)
暫時無法取得訂價和供貨情況
USP
冰醋酸, United States Pharmacopeia (USP) Reference Standard
暫時無法取得訂價和供貨情況