HPLC-MS/MS法同时检测牛奶中17种β2-受体激动剂和β-受体阻滞剂残留

A method for the determination of 17 β₂-agonists and β-blockers in milk was developed by solid-phase extraction(SPE) and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The samples were extracted with acetontrile and cleaned with an Oasis MAX SPE cartridge, after protein precipitation with trichloracetate. The analytics were quantified by HPLC-ESI-MS/MS operating in positive multiple-reaction mode(MRM). Recoveries of 17 compounds range from 61.6 % to 134.3%, and the RSDs are less than 25%. LOD and LOQ of the analytics upon the method range from 0.024 to 3.960 μg kg^－1 and from 0.068 to 13.200 μg kg^－1.     

液相色谱-串联质谱法测定小麦、麦秸和土壤中氟唑磺隆及其代谢物残留

An analytical method was developed to measure the residues of Flucarbazone-sodium and its Metabolites in wheat grain, straw, and soil by HPLC-MS/MS. The lowest level of method validation (LLMV) is 0.01 mg•kg^－1 for Flucarbazone-sodium and its Metabolites in straw and soil, and 0.005 mg•kg^－1 in wheat grain. The average fortified recoveries are between 74% and 103% with a relative standard deviation (RSD) between 3.4% and 16.3%.     

气相色谱-质谱法测定奶粉中的三聚氰胺

Melamine in milk power was determined by gas chromatography-mass spectrometer(GC/MS) made in china. The results show that the method has a good liner range between 0.005 mg•L^－1 and 2 mg•L^－1, R2 is 0.999 7. The limit of detection is 0.001 mg•L^－1, the quantitative detection limit is 0.02 mg•kg^－1. The recovery for melamine is in the range of 94％-102％. The method has good sensitivity, selectivity and repeatability, which has been applied to the determination of melamine in milk powder.     

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％.     

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.     

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.     

液相色谱-串联质谱法测定Beagle犬血浆中罗替戈汀的浓度

The rotigotine in beagle dog plasma was determined by liquid chromatographic-tandem mass spectrometry. The method of HPLC-MS/MS was used, and detection was performed on a tandem spectrometry in multiple reaction monitoring(MRM) mode. The standard curves are linear in the range of 0.025-12.5 μg L^－1, and the recovery is 89%-91%, the intra-day and the inter-day precision are less than 5.6% and 6.8%, respectively. The low limit of quantification(LLOQ) is 0.025 μg L^－1. The specificity is good and sensitive, so this method is suitable for the parmacokinetical research of rotigotine.     

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.     

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.     

超高效液相色谱-串联质谱法测定动物源性食品中性激素多组分残留

A rapid, specific and highly sensitive method for the simultaneous determination of seven sex hormones residueing in animal product was developed, which was based on UPLC-MS/MS under positive mode using electrospray ionization(ESI) source. ZnCl₂ was added to the extract solution to remove fat, and then target compounds were purified by LC-C₁₈ and LC-NH₂ solid phase extraction cartridge. Average recoveries for the seven sex hormone(spiked at the levels of 4 μg kg^－1 in fish product) range from 88% to 105%，with relative standard deviations between 4.3% and 24%.