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.     

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.     

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.     

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.     

HPLC-ICPMS测定面粉样品中溴酸盐与溴化物

A simple quantitative method of BrO₃^－ and Br^－ in flour using high performance liquid chromatography -inductively coupled plasma mass spectrometry was established. The detection limits for BrO₃^－ and Br^－(counted as Br) were 0.052 µg•L^－1 and 0.048 µg•L^－1, respectively. Three sample preparation methods were compared including ultrasonic method, bathing method and oscillation method. Oscillation method was selected finally. The recoveries of BrO₃^－ and Br^－ are between 93% and 112%.     

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.     

解吸附-电喷雾离子化质谱方法快速检测啤酒中的甲基乙二醛

A desorption electrospray ionization mass spectrometry(DESI-MS) method was developed to determine methylglyoxal(MG) present in beers. This method utilized 1,2-diamino-4,5-dimethoxybenzene to convert MG to 6,7-dimethoxy-2-methylquinoxaline, and then determined the derivative by DESI-MS. 1×10^－5 mol•L^－1 MG in water and 5×10－5 mol•L^－1 MG in Yan Jing beer can be determined using this method. This time-saving method may provide a way for high-throughput analysis of MG in beverages.     

电喷雾萃取电离快速测定尿样中的沙丁胺醇

A method for rapid determination of salbutamol in human urine was proposed in this study. The effects of the operation parameters, including spray voltage, temperature of the heating capillary, flow rate of extracting solvent, etc. on analysis performance were systematically investigated. Under the optimized experimental conditions, salbutamol in human urine is detected rapidly without any sample preparation with a detection limit lower than 0.1 μg•L^－1.     

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.