A liquid chromatography with tandem mass spectrometry（LC-MS/MS） method has been developed and validated for the measurement of sunitinib in rabbit plasma. After protein precipitation with acetonitrile, samples were ...A liquid chromatography with tandem mass spectrometry（LC-MS/MS） method has been developed and validated for the measurement of sunitinib in rabbit plasma. After protein precipitation with acetonitrile, samples were analyzed on a Zorbax Extend-C18 column（150 mm×4.6 mm, 5μm）. The mobile phase consisted of a mixture of acetonitrile and deionized water（containing 0.05% formic acid） at a ratio of 27：73（v/v）, and the flow rate was set at 0.8 mL /min. The column temperature was maintained at 30 oC. The LC eluate was detected by an electrospray ionization（ESI） source operated in the positive ion mode, and quantification was conducted using MRM of the transitions m/z 399.24→283.01 and m/z 415.19→178.00 for sunitinib and internal standard（IS, diltiazem hydrochloride）, respectively. The calibration curve was linear in the range of 2–600 ng/m L. The lower limit of quantification was 2 ng/mL. The method also exhibited satisfactory results in terms of sensitivity, specificity, accuracy（with relative error ranging from –4.0% to 1.1%）, precision（with intra- and inter-day relative standard deviations ranging from 2.8% to 9.5%）, matrix effect, recovery as well as stability. Taken together, our newly developed method was reliable to monitor sunitinib concentrations in rabbit plasma.展开更多
In order to obtain nanomaterials with superparamagnetism and high saturation magnetization, Mn-doped or Zn-doped superparamagnetic ferrite nanoclusters(Mn-FNs or Zn-FNs) were prepared by microwave-assisted solvotherma...In order to obtain nanomaterials with superparamagnetism and high saturation magnetization, Mn-doped or Zn-doped superparamagnetic ferrite nanoclusters(Mn-FNs or Zn-FNs) were prepared by microwave-assisted solvothermal method in this study. Preliminary investigations were performed by transmission electron microscopy(TEM) and dynamic light scattering(DLS) instrument to observe the morphology and measure the particle size, respectively. Afterwards, Zn-FNs were chosen to be further characterized in vitro due to their better morphology and dispersity than Mn-FNs. The subsequent characterizations included crystalline phase, metal content and magnetic properties by X-ray diffractometer(XRD), inductively coupled plasma-mass spectrometry(ICP-MS) and vibrating sample magnetometer(VSM), respectively. The results showed that Zn-FNs had a cluster-like structure assembled by multiple nanoparticles. Zn-FNs were spherical in shape with good dispersity and relatively uniform particle size. Zn was successfully doped in Zn-FNs which demonstrated spinel structure and excellent magnetic properties. Therefore, Zn-FNs had a favorable application prospect as a new type of magnetic nanomaterial.展开更多
In the present study, we developed and validated a simple and sensitive gradient elution liquid chromatography tandem mass spectrometry （LC-MS/MS） method for quantification of doxorubicin in rabbit plasma. Daunorubi...In the present study, we developed and validated a simple and sensitive gradient elution liquid chromatography tandem mass spectrometry （LC-MS/MS） method for quantification of doxorubicin in rabbit plasma. Daunorubicin was used as an internal standard （IS）. The doxorubicin and IS were extracted with ethyl acetate from plasma samples. The chromatographic separations were achieved on a C18 column （2.1 mm×50 mm, 2.5μm） configured with a C18 guard column （2.1 mm×10 mm, 2.5 μm）. The mobile phase of 0.1% formic acid-water solution and acetonitrile was delivered using a gradient elution program at a flow rate of 0.4 mL/min. The temperature for column was maintained at 40 ℃. The electrospray ionization （ESI） source was operated in the positive ion mode, and the quantification was conducted using multiple reaction monitoring （MRM） of the transitions m/z 544.07→396.96 and m/z 528.06→321.05 for doxorubicin and IS, respectively. The calibration curve of doxorubicin was linear （r 〉 0.999） within the range of 2-600 ng/mL. The lower limit of quantification was 2 ng/mL. The relative errors of intra-day and inter-day accuracies ranged from -2.48% to 0.18% and from -3.78% to 1.94%, respectively. The relative standard deviations of intra-day and inter-day precisions were less than 8.65% and 6.41%, respectively. The method exhibited satisfactory results in terms of specificity, sensitivity, matrix effect, recovery and stability. The newly developed LC-MS/MS method was reliable to monitor doxorubicin concentrations in rabbit plasma.展开更多
文摘A liquid chromatography with tandem mass spectrometry（LC-MS/MS） method has been developed and validated for the measurement of sunitinib in rabbit plasma. After protein precipitation with acetonitrile, samples were analyzed on a Zorbax Extend-C18 column（150 mm×4.6 mm, 5μm）. The mobile phase consisted of a mixture of acetonitrile and deionized water（containing 0.05% formic acid） at a ratio of 27：73（v/v）, and the flow rate was set at 0.8 mL /min. The column temperature was maintained at 30 oC. The LC eluate was detected by an electrospray ionization（ESI） source operated in the positive ion mode, and quantification was conducted using MRM of the transitions m/z 399.24→283.01 and m/z 415.19→178.00 for sunitinib and internal standard（IS, diltiazem hydrochloride）, respectively. The calibration curve was linear in the range of 2–600 ng/m L. The lower limit of quantification was 2 ng/mL. The method also exhibited satisfactory results in terms of sensitivity, specificity, accuracy（with relative error ranging from –4.0% to 1.1%）, precision（with intra- and inter-day relative standard deviations ranging from 2.8% to 9.5%）, matrix effect, recovery as well as stability. Taken together, our newly developed method was reliable to monitor sunitinib concentrations in rabbit plasma.
基金National Natural Science Foundation of China(Grant No.81571779).
文摘In order to obtain nanomaterials with superparamagnetism and high saturation magnetization, Mn-doped or Zn-doped superparamagnetic ferrite nanoclusters(Mn-FNs or Zn-FNs) were prepared by microwave-assisted solvothermal method in this study. Preliminary investigations were performed by transmission electron microscopy(TEM) and dynamic light scattering(DLS) instrument to observe the morphology and measure the particle size, respectively. Afterwards, Zn-FNs were chosen to be further characterized in vitro due to their better morphology and dispersity than Mn-FNs. The subsequent characterizations included crystalline phase, metal content and magnetic properties by X-ray diffractometer(XRD), inductively coupled plasma-mass spectrometry(ICP-MS) and vibrating sample magnetometer(VSM), respectively. The results showed that Zn-FNs had a cluster-like structure assembled by multiple nanoparticles. Zn-FNs were spherical in shape with good dispersity and relatively uniform particle size. Zn was successfully doped in Zn-FNs which demonstrated spinel structure and excellent magnetic properties. Therefore, Zn-FNs had a favorable application prospect as a new type of magnetic nanomaterial.
基金National Natural Science Foundation of China（ Grant No.81571779）.
文摘In the present study, we developed and validated a simple and sensitive gradient elution liquid chromatography tandem mass spectrometry （LC-MS/MS） method for quantification of doxorubicin in rabbit plasma. Daunorubicin was used as an internal standard （IS）. The doxorubicin and IS were extracted with ethyl acetate from plasma samples. The chromatographic separations were achieved on a C18 column （2.1 mm×50 mm, 2.5μm） configured with a C18 guard column （2.1 mm×10 mm, 2.5 μm）. The mobile phase of 0.1% formic acid-water solution and acetonitrile was delivered using a gradient elution program at a flow rate of 0.4 mL/min. The temperature for column was maintained at 40 ℃. The electrospray ionization （ESI） source was operated in the positive ion mode, and the quantification was conducted using multiple reaction monitoring （MRM） of the transitions m/z 544.07→396.96 and m/z 528.06→321.05 for doxorubicin and IS, respectively. The calibration curve of doxorubicin was linear （r 〉 0.999） within the range of 2-600 ng/mL. The lower limit of quantification was 2 ng/mL. The relative errors of intra-day and inter-day accuracies ranged from -2.48% to 0.18% and from -3.78% to 1.94%, respectively. The relative standard deviations of intra-day and inter-day precisions were less than 8.65% and 6.41%, respectively. The method exhibited satisfactory results in terms of specificity, sensitivity, matrix effect, recovery and stability. The newly developed LC-MS/MS method was reliable to monitor doxorubicin concentrations in rabbit plasma.
