目的:运用反相高效液相色谱联合荧光检测器法测定盐酸氟桂利嗪片中盐酸氟桂利嗪的含量及含量均匀度。方法:采用DiamonsilTMC18柱(250mm×4.6mm,5耻m).以甲醇:0.02mol/L磷酸二氢铵(0.1%三乙胺,磷酸调pHi3.0)(70:30...目的:运用反相高效液相色谱联合荧光检测器法测定盐酸氟桂利嗪片中盐酸氟桂利嗪的含量及含量均匀度。方法:采用DiamonsilTMC18柱(250mm×4.6mm,5耻m).以甲醇:0.02mol/L磷酸二氢铵(0.1%三乙胺,磷酸调pHi3.0)(70:30)为流动相.流速为ImL/min,激发波长260nm.发射波长310nm,柱温为25℃,进样体积10μL,进行了方法学考察和盐酸氟桂利嗪的含量及均匀度测定。结果:盐酸氟桂利嗪在6.1~122ng(r=0.9992)范围内呈良好的线性关系.平均回收率为100.07%(RSD=1.38%):LOD(1imit of detection)和LOQ(1imit of quantification)分别为2.44ng、8.13ng;盐酸氟桂利嗪片三批样品的平均标示量分别为98.27%、98.79%、99.89%,其含量均匀度A+I.8S分别为5.644、4.194、7.160,均小于15。结论:该方法快速、准确,无杂质干扰.可为盐酸氟桂利嗪片的质量标准的建立与完善提供科学依据并指导临床合王早用药.展开更多
Background: Sialic acids are a family of ninecarbon sugar compounds with carboxylic acyl derivatives. It exists in bacteria, fish, mammals and other living organisms, participates in and regulates many important life ...Background: Sialic acids are a family of ninecarbon sugar compounds with carboxylic acyl derivatives. It exists in bacteria, fish, mammals and other living organisms, participates in and regulates many important life events, such as cell recognition, membrane flow, endocytosis and so on. Sialic acid is usually located in the outermost layer of the sugar part of the cell membrane and the key positions of secreted glycoconjugates (glycolipids, glycoprotein and lipopolysaccharide). Sialic acid (Sia) is an important material foundation for variety of the structure and founction of glycoconjugates. Sia has been known as nearly 50 members, including N-acetylneuraminic acid (Neu5Ac), N-glycoulylneuraminic acid (Neu5Gc) and deaminoneuraminic acid (KDN) as its core monomer. The rest of the sialic acids are derived from these three monomers. The contents of Sia in Chinese food products are unknown. Objective: To determine the contents of Sia in raw and cooked red meat, seafood, poultry and so on. Design: The following food products were purchased from a Chinese supermarket: pork, beef, lamb, salmon, cod, tuna, cow milk, cheese, butter, duck, chicken and chicken eggs. Human milk was collected from Xiamen Maternity and Child Health Care Hospital (Xiamen, China). All tissues were homogenized and hydrolyzed with 0.05 M, 0.1 M and 0.2 M TFA for 150 min at 80°C in dark, respectively. The concentrations of Neu5Ac, Neu5Gc and KDN were determined by using HPLC with fluorescence detector. Results: The contents of total Sia (μg/g tissue or μg/mL liquid sample) in Chinese raw meat were highest in lamb (269.60), followed by pork (254.88), duck (200.63), chicken (162.86) and beef (88.03). The percentages of Neu5Gc were 36.08%, 26.48%, 0%, 0% and 28.40%, respectively. Cod contained higher levels of Sia (171.63) than salmon (104.43) and tuna (77.98). Only Neu5Ac was 50 found in detected aquatic product. Egg yolk contained the highest level of Sia (682.04), and a higher level of Sia (390.67) was found in the egg white. Also our result showed that human milk contained extremely high level of Sia (602.55). Neu5Ac was the predominant form of Sia in all the deteced samples. KDN was found in cow milk only among the samples, the content was 1.14 μg/g. Conclusion: The highest content of Sia in examined Chinese foods was found in 56 eggs, followed by lamb, pork, duck, cod, chicken, salmon, beef and tuna. Knowledge of the Sia content in conventional foods may help us to better understand possible medical disorders involving the uptake of the “non-human” Neu5Gc from our diet.展开更多
文摘目的:运用反相高效液相色谱联合荧光检测器法测定盐酸氟桂利嗪片中盐酸氟桂利嗪的含量及含量均匀度。方法:采用DiamonsilTMC18柱(250mm×4.6mm,5耻m).以甲醇:0.02mol/L磷酸二氢铵(0.1%三乙胺,磷酸调pHi3.0)(70:30)为流动相.流速为ImL/min,激发波长260nm.发射波长310nm,柱温为25℃,进样体积10μL,进行了方法学考察和盐酸氟桂利嗪的含量及均匀度测定。结果:盐酸氟桂利嗪在6.1~122ng(r=0.9992)范围内呈良好的线性关系.平均回收率为100.07%(RSD=1.38%):LOD(1imit of detection)和LOQ(1imit of quantification)分别为2.44ng、8.13ng;盐酸氟桂利嗪片三批样品的平均标示量分别为98.27%、98.79%、99.89%,其含量均匀度A+I.8S分别为5.644、4.194、7.160,均小于15。结论:该方法快速、准确,无杂质干扰.可为盐酸氟桂利嗪片的质量标准的建立与完善提供科学依据并指导临床合王早用药.
文摘Background: Sialic acids are a family of ninecarbon sugar compounds with carboxylic acyl derivatives. It exists in bacteria, fish, mammals and other living organisms, participates in and regulates many important life events, such as cell recognition, membrane flow, endocytosis and so on. Sialic acid is usually located in the outermost layer of the sugar part of the cell membrane and the key positions of secreted glycoconjugates (glycolipids, glycoprotein and lipopolysaccharide). Sialic acid (Sia) is an important material foundation for variety of the structure and founction of glycoconjugates. Sia has been known as nearly 50 members, including N-acetylneuraminic acid (Neu5Ac), N-glycoulylneuraminic acid (Neu5Gc) and deaminoneuraminic acid (KDN) as its core monomer. The rest of the sialic acids are derived from these three monomers. The contents of Sia in Chinese food products are unknown. Objective: To determine the contents of Sia in raw and cooked red meat, seafood, poultry and so on. Design: The following food products were purchased from a Chinese supermarket: pork, beef, lamb, salmon, cod, tuna, cow milk, cheese, butter, duck, chicken and chicken eggs. Human milk was collected from Xiamen Maternity and Child Health Care Hospital (Xiamen, China). All tissues were homogenized and hydrolyzed with 0.05 M, 0.1 M and 0.2 M TFA for 150 min at 80°C in dark, respectively. The concentrations of Neu5Ac, Neu5Gc and KDN were determined by using HPLC with fluorescence detector. Results: The contents of total Sia (μg/g tissue or μg/mL liquid sample) in Chinese raw meat were highest in lamb (269.60), followed by pork (254.88), duck (200.63), chicken (162.86) and beef (88.03). The percentages of Neu5Gc were 36.08%, 26.48%, 0%, 0% and 28.40%, respectively. Cod contained higher levels of Sia (171.63) than salmon (104.43) and tuna (77.98). Only Neu5Ac was 50 found in detected aquatic product. Egg yolk contained the highest level of Sia (682.04), and a higher level of Sia (390.67) was found in the egg white. Also our result showed that human milk contained extremely high level of Sia (602.55). Neu5Ac was the predominant form of Sia in all the deteced samples. KDN was found in cow milk only among the samples, the content was 1.14 μg/g. Conclusion: The highest content of Sia in examined Chinese foods was found in 56 eggs, followed by lamb, pork, duck, cod, chicken, salmon, beef and tuna. Knowledge of the Sia content in conventional foods may help us to better understand possible medical disorders involving the uptake of the “non-human” Neu5Gc from our diet.