Browsing by Author "Malebo Hamisi M."
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Item A HPLC-MS/MS method for screening of selected antibiotic adulterants in herbal drugs(The Royal Society of Chemistry, 2022) Mwankuna Christopher Johnson; Uwamaliya Grâce Ange; Mariki Eliapenda Elisante; Mabiki Faith; Malebo Hamisi M.; Mdegela Robinson; Styrishaveb BjarneThe use of herbal products adulterated with conventional drugs increases the risk of developing microbial resistance and causes herb-to-drug interaction, leading to severe clinical consequences. The complex nature of herbal products has been a challenge for the unambiguous identification of adulterants. The improved analytical selectivity and sensitivity of hyphenated techniques such as high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) enable the confirmatory screening of adulterants in herbal products. Simultaneous screening of adulterants is necessary and efficient because it has been established that more than one chemical adulterant may be present in one herbal product. An HPLC-MS/MS method for the simultaneous detection and quantification of amoxicillin, ampicillin, metronidazole, ciprofloxacin, sulfamethoxazole, and trimethoprim in powdered herbal drugs was developed. Deuterated metronidazole-d3, trimethoprim-d3, ciprofloxacin-d8, and sulfamethoxazole-d4 were used as internal standards (ISs). For each analyte, two transitions were monitored using protonated molecules as precursor ions. The extraction of analytes from herbal products was performed using a simple methanol : water : formic acid (90 : 10 : 0.05, v/v) extraction solvent. Chromatographic separation was done in a gradient of 0.01% formic acid in methanol and 0.01% formic acid in MilliQ water. The calibration curves were linear (r2 $ 0.996) over the range of 0.005–2.5 mg mL 1 for all compounds except metronidazole, whose range was 0.005–1 mg mL 1. The limit of detection (LOD) ranged from 0.012 to 0.046 mg mL 1, while the limit of quantification (LOQ) ranged from 0.066 to 0.153 mg mL 1. The accuracy, expressed as the recovery of spiked herbal products, ranged from 45% to 114%. The precision, expressed as relative standard deviation (RSD) at two concentration levels, ranged from 1.6% to 15.9%. The matrix effect expressed as the matrix factor (MF) ranged from 0.79 to 0.92. The developed method was applied to powder herbal products purchased in Tanzania. Amoxicillin, ampicillin, trimethoprim, sulfamethoxazole, and ciprofloxacin were not detected in all samples. Metronidazole was detected in eight samples with the highest concentration of 1.38 mg g 1. The developed method is suitable for the detection of all the studied antibiotic adulterants in herbal products. Quantification can be performed for all the compounds except ciprofloxacin due to its lower recovery.Item Optimization of HPLC–MS/MS method for determination of antimalarial adulterants in herbal products(SPRINGER, 2023-01-12) Mwankuna Christopher J.; Kiros Feven; Mariki Eliapenda E.; Mabiki Faith P.; Malebo Hamisi M.; Mdegela Robinson H.; Styrishave BjarneThe use of herbal products is booming all over the world because of being believed as safer than conventional drugs and free of side effects. However, there are untrustworthy manufacturers who adulterate herbal products by adding conventional drugs which might eventually lead to microbial resistance and herb-to-drug interactions. There is a need to develop methods for detecting adulterants in herbal products. A high performance liquid chromatography-tandem mass spectrometry (HPLC– MS/MS) method for simultaneous identification and determination of conventional antimalarials (chloroquine, quinine, sulfadoxine, pyrimethamine, mefloquine, lumefantrine, amodiaquine, artemisinin, dihydroartemisinin, artesunate and artemether) in herbal products was developed. Stable isotopically labelled compounds (artemether-d3, quindine-d3, and sulfadoxine-d3) were used as internal standards (ISs) for quantitative analysis. Extraction of analytes was performed using methanol: water: formic acid (90:10:0.1, v/v) and chromatographic separation was done in a gradient mode using mobile phase A: Ultrapure water containing 0.1% formic acid and 1 mM ammonium formate and mobile phase B: Acetonitrile/ methanol (50:50) containing 0.1% formic acid and 1 mM ammonium formate. The calibration curves were linear (r2 ≥ 0.991) over the range of 0.001–0.3 μg mL−1 for all compounds. The limit of detection (LOD) ranged from 0.002 to 0.02 μg mL−1 while the limit of quantification (LOQ) ranged from 0.006 to 0.08 μg mL−1. Accuracy, expressed as recovery of spiked herbal products ranged from 52 to 128%. The precision, expressed as percent relative standard deviation (%RSD) at two concentration levels, ranged from 1.0 to 13.8%. The matrix effect expressed as the matrix factor (MF) ranged from 0.77 to 0.97. The developed method was used to identify and quantify conventional antimalarials in herbal product samples from Tanzania. Ten out of 50 herbal products were found to contain amodiaquine, sulfadoxine, pyrimethamine, mefloquine, dihydroartemisinin, artemether and lumefantrine. The developed method is considered a valuable tool for getting a better understanding of the adulteration of conventional antimalarials in herbal products.