目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-py...目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。展开更多
A total of 16 Friesian cows were used in the study to determine the peripheral concentration of hydroxyproline(HYPRO) and 3 methyl histidine(3 MEHIS).The objectives of the experiment were to find out the relationshi...A total of 16 Friesian cows were used in the study to determine the peripheral concentration of hydroxyproline(HYPRO) and 3 methyl histidine(3 MEHIS).The objectives of the experiment were to find out the relationship between collagen and myosin degradation and uterine involution in the postpartum cow.The results showed tht the mean concentrations of HYPRO and 3 MEHIS were 13.47±2.38 and 18.35±2.77 n mole/mL,respectively,for the cows during the days 60～90 postpartum.And for the cows immediately after calving the concentrations of HYPRO and 3 HEHIS reduced from 34.29 and 28.06 nmole/mL on the day one after calving to the normal lever of 13.23 and 17.97 n mole on the day 50 postpartum,respectively.There was a good correlation between the peripheral concentrations of both HYPRO and 3 MEHIS and the diameters of the involuting uterus(r=0.8128).展开更多
The urinary concentrations of hydroxyproline (HYPRO)and 3 -methyl histidine (3 - MEHIS) were de- termined in 16 Chinese-Holstein cows. The objectives of the experiment were to find out thhe relationship between collag...The urinary concentrations of hydroxyproline (HYPRO)and 3 -methyl histidine (3 - MEHIS) were de- termined in 16 Chinese-Holstein cows. The objectives of the experiment were to find out thhe relationship between collagen and myosin ddegradation and uterine involution in the postpartum cow. The results in the experiment showed that the mean concentrations of HYPRO and 3-MEHIS were 138.32±22.99 and 37.09 ±3.90 nmol·mL-1,respectively,for the cows during the days between 60-90 postpartum,and for the cows immediately after calving the concentrations of HYPRO and 3 -MEHIS reduced from 284.30 and 65.48 nmol ·mL-1 on the day one after calving to the normal level of 109.18 and 33.51 nmol·mL^-1 on the day 50 post- partum,respectively. There was a good correlation between the urinary concentrations of both HYPRO and 3 -MEHIS and the diameters of the involuting uterus (r = 0. 79).展开更多
文摘目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。
基金The project is supported financially by Heilongjiang and Chinese ntional and Scientific fund
文摘A total of 16 Friesian cows were used in the study to determine the peripheral concentration of hydroxyproline(HYPRO) and 3 methyl histidine(3 MEHIS).The objectives of the experiment were to find out the relationship between collagen and myosin degradation and uterine involution in the postpartum cow.The results showed tht the mean concentrations of HYPRO and 3 MEHIS were 13.47±2.38 and 18.35±2.77 n mole/mL,respectively,for the cows during the days 60～90 postpartum.And for the cows immediately after calving the concentrations of HYPRO and 3 HEHIS reduced from 34.29 and 28.06 nmole/mL on the day one after calving to the normal lever of 13.23 and 17.97 n mole on the day 50 postpartum,respectively.There was a good correlation between the peripheral concentrations of both HYPRO and 3 MEHIS and the diameters of the involuting uterus(r=0.8128).
基金supported financially by Heilongjiang(C- 9702)and Chinese National (39870572)Natural and Scicntificfunds.
文摘The urinary concentrations of hydroxyproline (HYPRO)and 3 -methyl histidine (3 - MEHIS) were de- termined in 16 Chinese-Holstein cows. The objectives of the experiment were to find out thhe relationship between collagen and myosin ddegradation and uterine involution in the postpartum cow. The results in the experiment showed that the mean concentrations of HYPRO and 3-MEHIS were 138.32±22.99 and 37.09 ±3.90 nmol·mL-1,respectively,for the cows during the days between 60-90 postpartum,and for the cows immediately after calving the concentrations of HYPRO and 3 -MEHIS reduced from 284.30 and 65.48 nmol ·mL-1 on the day one after calving to the normal level of 109.18 and 33.51 nmol·mL^-1 on the day 50 post- partum,respectively. There was a good correlation between the urinary concentrations of both HYPRO and 3 -MEHIS and the diameters of the involuting uterus (r = 0. 79).
