Zhongguo xue xi chong bing fang zhi za zhi = Chinese journal of schistosomiasis control · 2018
[Development of a novel method for UPLC-QTOF-MS analysis of anti-schistosomiasis heterocyclic compounds].
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Yang Ye, Ren-Jie Hui, Bai-Nian Feng
Аннотация
OBJECTIVE: To develop an ultra-performance liquid chromatography/quadrupole-time of flight mass spectrometry (UPLC-QTOF-MS) method for the determination of an oxadiazole-2-oxide heterocyclic compound F-2015-14.
METHODS: Mouse plasma and liver homogenate specimens were extracted with ethyl acetate and chromatographed on a Waters CORTECS column (C18, 1.6 μm, 2.1 mm × 150 mm) by using a mobile phase of 10% acetonitrile-0.1% formic acid with by a volume fractionation by gradient elution. Then, UPLC-QTOF-MS was performed to determine F-2015-14 in mouse plasma and liver homogenate specimens.
RESULTS: The linearity of F-2015-14 in plasma ranged from 12.5 to 250 mg/mL with a correlation coefficient of 0.990 and a detection limit of 8.8 mg/mL. F-2015-14 in liver homogenates ranged from 12.5 to 250 mg/mL. The linearity was good with a correlation coefficient of 0.992 and a limit of detection of 5.6 mg/mL. If the concentration of plasma and liver homogenate specimens was 12.5 mg/mL, the accuracy and the matrix effect were 80% to 120%, and the inter-day and intra-day precision was within 20%. If the concentrations of plasma and liver homogenate specimens were 100 mg/mL and 200 mg/mL, the accuracy and the matrix effect were 85% to 115%, and the inter-day and intra-day precision was within 15%.
CONCLUSIONS: The UPLC-QTOF-MS established in this study has a high sensitivity and good reproducibility for the determination of F-2015-14, which provides bases for the development of novel anti-schistosomiasis drugs.
METHODS: Mouse plasma and liver homogenate specimens were extracted with ethyl acetate and chromatographed on a Waters CORTECS column (C18, 1.6 μm, 2.1 mm × 150 mm) by using a mobile phase of 10% acetonitrile-0.1% formic acid with by a volume fractionation by gradient elution. Then, UPLC-QTOF-MS was performed to determine F-2015-14 in mouse plasma and liver homogenate specimens.
RESULTS: The linearity of F-2015-14 in plasma ranged from 12.5 to 250 mg/mL with a correlation coefficient of 0.990 and a detection limit of 8.8 mg/mL. F-2015-14 in liver homogenates ranged from 12.5 to 250 mg/mL. The linearity was good with a correlation coefficient of 0.992 and a limit of detection of 5.6 mg/mL. If the concentration of plasma and liver homogenate specimens was 12.5 mg/mL, the accuracy and the matrix effect were 80% to 120%, and the inter-day and intra-day precision was within 20%. If the concentrations of plasma and liver homogenate specimens were 100 mg/mL and 200 mg/mL, the accuracy and the matrix effect were 85% to 115%, and the inter-day and intra-day precision was within 15%.
CONCLUSIONS: The UPLC-QTOF-MS established in this study has a high sensitivity and good reproducibility for the determination of F-2015-14, which provides bases for the development of novel anti-schistosomiasis drugs.