LC-MS/MS法测定犬血浆中脂质纳米粒10-羟基喜树碱浓度

10-hydroxycamptothecin，camptothecin analogue，is an antitumor agent that targets the nuclear enzyme topoisomerase I. 10-hydroxycamptothecin is injected by sodium salt form in clinic, and myelosuppression is the major toxicity. To enhance water solubility and reduce the toxicity, lipid nanoparticle which is water-soluble was designed. The quantitative analyses of liposomal and total 10-hydroxycamptothecin in dog plasma were developed and validated by liquid chromatographic-tandem mass spectrometry(LC-MS/MS). Two preparation procedures were developed to separate liposomal 10-hydroxycamptothecin, one was solid phase extraction, the other was liquid-liquid extraction. The analyte and internal standand(camptothecin) were separated on a Zorbax SB-C₁₈ column using the mobile phase consisting of V(acetonitrile):V(water):V(formic acid)＝70:30:0.2. Electropray ionization source of MS was applied and operated in positive ion mode. The peak area of the m/z 365→321 transition of 10-hydroxycamptothecin and that of m/z 349→305 transition of the IS were measured. The linear calibration curve for liposmal 10-hydroxycamptothecin is obtained in the concentration range of 1.00- 1 000μg L^－1, and that for total 10-hydroxycamptothecin is obtained in the concentration range of 1.00- 2 000μg L－1. The recoveries of solid phase extraction and liquid-liquid extraction methods are 48.1%-52.4% and 79.6%-83.0%, respectively. This validated LC-MS/MS assay is successfully applied to pharmacokinetic study of 10-hydroxycamptothecin loaded lipid nanoparticle in dogs after administration single dosages of 0.5, 1, 2 mg kg^－1 and multiple dosage of 1.0 mg kg^－1 d^－1 10-hydroxycamptothecin lipid nanoparticle.     

LC-MS/MS法定量测定人血浆中CPRC-127血药浓度

A sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric(LC-MS/MS) method for the determination of CPRC-127 in human plasma was developed and validated. The plasma was extracted using a liquid-liquid phase extraction(LLE), and the sample extract was injected onto the LC-MS/MS system. The limit of quantitation(LLOQ) for CPRC-127 is 0.5 μg•L^－1. This method allows the reproducible and accurate quantification with the concentration range of 0.5-1 000 μg•L^－1. This method can be applied to the quantitation of CPRC-127 in human plasma.     

LC-MS/MS法定量测定人血浆中TF及其代谢产物M1，M2

A sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric(LC-MS/MS) method for the simultaneous determination of TF and its metabolites M1 and M2 in human plasma were developed and validated. The plasma TF, M1, M2 were extracted using a solid phase extraction(SPE), and the sample extract was injected onto the LC-MS/MS system. The limits of quantitation(LLOQ) for TF, M1, M2 are 1 ng•L^－1. This method allowes the reproducible and accurate quantification with the concentration range of 1-500 ng•L^－1. This method can be applied to the quantitation of TF, M1, M2 in human plasma.     

液相色谱-串联质谱同时测定牛奶中10种蛋白同化激素的残留

A liquid chromatographic/tandem mass spectrometric (LC/MS/MS) multiresidue method for the simultaneous determination of 10 anabolic steroids (ASs) in whole milk were developed. Milk samples were extracted with methanol and the samples were then subjected to a clean-up procedure using liquid-liquid extraction (LLE) methods. The samples were analysed by LC/MS/MS. The limits of detection (LOD) of LC/MS/MS method used for testing the 10 ASs in whole milk ranged from 0.06 to 0.22 µg•L^－1, and the limits of quantification (LOQ) were from 0.12 to 0.54 µg•L^－1. Experiments on spiked samples of whole milk showed that at addition levels of 1.0, 2.0, 10 µg•L^－1 the average recoveries of the ASs were 24% to 86%, 25% to 91%, 31% to 71%, with relative standard deviations (RSDs) ranged from 12% to 37%, 5% to 20%, 10% to 16%, respectively.     

简易氢化物发生-ICP-MS法测定高纯钴中痕量的砷

A method for the determination of trace arsenic in high purity cobalt with hydride generation-ICP-MS was reported. Due to the interference of the oxide complex ions ⁵⁹Co¹⁶O^＋, the background concentration of ⁷⁵As is about 100 µg•L^－1 in 1 g•L^－1 cobalt solution, which lead to the impossibility of the direct analysis for the trace As in high purity cobalt. However, the As background concentration can be decreased to several µg•L^－1 if the simple HG system was applied and the 0.05 µg•g^－1 of determination limits can obtained with this method.     

HPLC-MS/MS法测花旗松素在Beagle犬血浆中的浓度及其药代动力学研究

A rapid, sensitive and selective method for the determination of taxifolin in Beagle dog plasma was described by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Resveratrol was used as internal standard (I.S.). MS detection and quantitation were done by mass spectrometer using selected reaction monitoring at m/z 303 and 285 [M－H]^－ for taxifolin, and m/z 227 and 185 [M－H]^－ for resveratrol. The calibration curve is linear (r＞0.998) from 2 to 1 000 μg L^－1, and the lower limit of quantification(LLOQ) is 2 μg L^－1.     

应用液相色谱-质谱联用技术同时测定花生中的黄曲霉毒素B1、B2、G1、G2

The aflatoxin B1, B2, G1, G2 in peanut were develop by LC-MS/MS. The mass spectrometer was operated in the positive ion mode using multiple reaction monitoring. The sample was extracted with methanol, and chromatographic separation was carried out on a MGIII-C₁₈ column(2.1 mm×150 mm×1.8 μm) with eluthic sion of V(acetonitrile):V(water)＝35:65. The limit of detection is 0.5 μg•L^－1, the limit of quantitation is 0.5 μg•kg^－1. The linear plots are between 0.5 μg•L^－1 and 25.0 μg•L^－1. Overall recoveries are between 88.3% and 99.2%, and RSD values are between 1.73％ and 3.75％.     

血液中曲马多的HPLC-MS/MS检验方法研究

The method for extraction and determination of tramadol was established by HPLC-MS/MS. Calibration curves are linear on injection of amounts range of 50-1 000 μg•L^－1. The limit of detection is 10 μg•L^－1, and the recovery is above 80% for Tramadol.     

液相色谱-串联质谱法测定玉米中伏马菌素B1

Fumonisin B1 in maize was determined by liquid chromatography/tandem mass spectrometry. The analysis was extracted from maize samples by acetonitrile-water-acetic acid 49:50:1(V/V/V). Raw extracts were evaporated to dryness and dissolved with mobile phase, chromatographyed on a C₁₈ column, and detection was performed on a triple quadrupole tandem mass spectrometry with electrospray ionization source. The method has a limit of quantification of 10 µg•kg^－1 in maize samples. The calibration curve is linear in the range of 1-500 µg•L^－1. The mean recovery ranges from 94 % to 104 %, and the relative standard derivations are lower than 9%. The method is sensitive and specific to be applied for determination of fumonisin B1 in maize samples.     

高效液相色谱-串联质谱法测定鸡蛋中三聚氰胺残留

An high-performance liquid chromatographic method with tandem mass spectrometry(HPLC-MS/MS) was developed for the determination of melamine residues in egg. In the method, the melamine residue was extracted with V(1% Trichloroacetic acid):V(methanol)＝1:1, cleaned-up with PCX solid phase extraction column, and concentrated to dry under nitrogen and redissolved in 1 mL dissolving solution. The solution was separated on a RP-HPLC column, and detected by HPLC-MS/MS with positive electrospray ionization(ESI＋) in multiple reaction monitoring(MRM) mode. Quantitation was carried out using an external standard method. The standard curves for all compounds are linear over the concentration range of 20-400 μg kg^－1 with correlation coefficients(r2) of 0.998 5. The recoveries of melamine from egg samples spiked with the concentration levels at 50, 100, 200 μg kg^－1 are range of 87.0%, 96.8%, 94.4%. The limits of detection for the method are 3 μg kg^－1. The limits of quantification for the method are 10 μg kg^－1. The results show that the established method is of simplicity, rapidity, high sensitivity, good reproducibility and better selectivity. The method is quite fit for identification and determination of melamine in egg.