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Validation of a straightforward high performance liquid chromatographic method for morphine quantitation.

ABSTRACT: Morphine is illegal to use unless it is prescribed by a medical doctor. This compound is commonly abused in the form of illicit heroin.An easy-to-use method for determining morphine in illicit heroin using high performance liquid chromatography-photodiode array detector (HPLC-PDA) was developed. With the aid of 50:50 acetonitrile:ammonium formate, this target compound traveling in a pentafluorophenyl (PFP) column was successfully separated from other compounds frequently present in the heroin matrix.The method was precise with an intra-day relative standard deviation (RSD) ≤ 0.8% and inter-day RSD < 5%. It was able to detect as low as 0.001 mg/mL morphine. The detector's response was linear (R2 > 0.999) and reliable for morphine quantitation from 0.005 up to 1 mg/mL. Through recovery studies, accuracy of the method was averagely estimated to be 89.54-101.91%.This method saves time in terms of mobile phase preparation and cuts cost by excluding additional purchase of expensive chemicals. More importantly, it proves to be able to determine the target analyte with sufficient accuracy and precision.

SUBMITTER: Chan KW

PROVIDER: S-EPMC5514187 | biostudies-other | 2017

REPOSITORIES: biostudies-other

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Project description:BackgroundThe non-nucleoside reverse transcriptase inhibitor dapivirine has been evaluated as a topical microbicidal agent to prevent HIV-1 acquisition. Several clinical trials have evaluated the pharmacokinetics of dapivirine when administered as a 25-mg intravaginal ring. Recent studies have focused on the distribution of dapivirine into breast milk. Drug distribution during lactation and breastfeeding can have implications in terms of infant drug exposure. Thus, sensitive bioanalytical tools are required to characterize the pharmacokinetics of dapivirine in breast milk.MethodsWhole breast milk was spiked with dapivirine and internal standard. Lipid content was disrupted via pre-treatment with n-hexane, and supernatants were subjected to solid phase extraction. Extracted materials were subjected to liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis. Separation occurred using a Waters BEH C8, 50 × 2.1 mm UPLC column with a 1.7 µm particle size and dapivirine was detected on an API 5000 mass analyzer. Methods were validated in accordance with FDA Bioanalytical Method Validation recommendations.ResultsThe analytical method was optimized for dapivirine extraction from breast milk. The analytical measuring range of the assay was 10-1000 pg/mL. Calibration curves were generated via weighted linear regression of standards. Intra- and inter-assay precision and accuracy studies demonstrated %CVs ≤ 14.6% and %DEVs ≤ ±12.7%. Stability and matrix effects studies were also conducted and deemed acceptable. The method was applied to a previously reported phase 1 clinical trial and demonstrated appropriate performance in the quantitation of dapivirine in breast milk samples from lactating women.ConclusionsAn ultrasensitive LC-MS/MS assay has been developed and validated for the quantitation of dapivirine in breast milk. The described method meets validation acceptance criteria and has been applied to a phase 1 clinical trial.

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Validation of a straightforward high performance liquid chromatographic method for morphine quantitation.

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