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.     

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％.     

ICP-MS法测定人尿样中15种微量稀土元素含量

Urine samples were collected in the morning and were stored frozen at −20 ℃ until analysed. The samples were wet digested by HNO₃＋HCLO₄ before determination. The solution was directly analyzed by ICP-MS for the determination of Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in human urine with rhenium internal standard calibration. The detection limits were 0.1-2.1 ng•L^－1. Certified reference material of human hair GBW 09101a was analyzed by the described method. The analytical values of the certified reference material showed closed agreement with the reference values.     

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.     

钚气溶胶直接进样ICP-MS快速分析技术-6级高效过滤器后钚气溶胶的定量

A technique for fast analysis of plutonium in airborne aerosol was developed with directly sampling ICP-MS in this laboratory. And the Pu-242 aerosol particle addition calibration method was established. The nebulized Pu-242 solution aerosol was quantitatively mixed with the airborne aerosol and then introduced into ICP-MS. The results show that the detection limit for Pu-239 concentration is down to 1.4×10^－6 Bq·L^－3. The airborne aerosol sample after through a high efficiency particulate air (HEPA) filter with six stages (efficiency per stage 99.95%) was analyzed using this technique, the plutonium concentration determined is 3×10^－4 Bq·L^－3. However plutonium could not be detected when sampling using HEPA filter at same situation, airborne aerosol also could not be detected at same situation with Condensation Particle Counter (CPC). This result shows there were some tiny plutonium particulates which passed through the six stages HEPA filter with airflow and could not be collected by the HEPA filter     

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.     

液相色谱-串联质谱法测定牛奶中舒巴坦和他唑巴坦

A triple quadrupole liquid chromatography tandem mass spectrometry method is presented for the quantitative determination and confirmation of salbactam and tazobactam, the inhibitors of β-lactamase in milk. Milk was extracted with methanol, and the extracts were analyzed by LC-MS/MS in negative mode. The LOQs of salbactam and tazobactam in milk are 10 μg•L^－1 and 100 μg•L^－1, respectively.     

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.