目的评估自动化磁珠法提取血清脂溶性维生素应用液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测的性能。方法收集200例临床剩余血清样本,采用自动化磁珠法提取血清中脂溶性维生素A,D_(2),D_(3),E和K...目的评估自动化磁珠法提取血清脂溶性维生素应用液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测的性能。方法收集200例临床剩余血清样本,采用自动化磁珠法提取血清中脂溶性维生素A,D_(2),D_(3),E和K;同时联合LC-MS/MS检测脂溶性维生素A,D_(2),D_(3),E和K的线性、定量限、精密度、正确度、携带污染率等性能指标以及基质效应。并比较此方法与传统萃取法检测结果的一致性。结果自动化磁珠法提取脂溶性维生素A,D_(2),D_(3),E和K线性相关系数均>0.99;五种物质的定量限分别为5,0.25,0.25,125和0.025ng/ml;批内精密度和批间精密度分别为0.66%~4.83%,0.15%~3.70%;平均加标回收率为87.05%~111.11%;基质效应为95.43%~99.07%;高-低值样本循环进样结果均值与低-低值样本循环进样结果均值之差,均小于低-低值样本循环进样结果均值的3s;统计学结果显示自动化磁珠法和传统萃取法提取的脂溶性维生素结果相关性良好(r>0.99),两种方法的检测结果无显著偏倚。结论自动化磁珠法提取脂溶性维生素的检测性能良好,有望提高样品通量和分析效率。展开更多
[Objectives]To develop a paeonol bead popping gum with hypoglycemic effect.[Methods]The paeonol bead popping gum was prepared by the"two-step method",that is,the pill core was prepared by the guttate pill me...[Objectives]To develop a paeonol bead popping gum with hypoglycemic effect.[Methods]The paeonol bead popping gum was prepared by the"two-step method",that is,the pill core was prepared by the guttate pill method,and then the coating was cured by sodium alginate solution and CaCl_(2) solution.The single factor method was used to determine the effects of PEG-4000:paeonol dosage ratio,dropper diameter,condensation time,dropping distance,melting temperature on the comprehensive score of paeonol guttate pill,and the effects of sodium alginate solution concentration,CaCl_(2) solution concentration,number of coating layers,drying time on the comprehensive score of popping gum.Finally,the optimal process was determined and verified by orthogonal experiment method.[Results]When the dosage ratio of PEG-4000:paeonol was 4∶1,the dropper diameter was 4 mm,the condensation time was 5 min,the dropping distance was 6 cm,and the melting temperature was 90℃,the quality of the prepared guttate pill was the optimal.When the concentration of sodium alginate solution was 0.02 g/mL,the concentration of CaCl_(2) solution was 0.25 g/mL,the number of coating layers was 3,and the drying time was 25 min,the appearance and comprehensive score of the obtained popping beads were the optimal.[Conclusions]This study is expected to provide some reference and basis for the development and utilization of hypoglycemic products of traditional Chinese medicine.展开更多
Alginate beads, often used for controlled release of enzymes and drugs, are usually produced by spraying sodium alginate liquid into a gelling agent using mechanical vibration nozzle or air jet. In this work an altern...Alginate beads, often used for controlled release of enzymes and drugs, are usually produced by spraying sodium alginate liquid into a gelling agent using mechanical vibration nozzle or air jet. In this work an alternative method of electro-spray was employed to form droplets with desired size from a highly viscous sodium alginate solution using constant DC voltage. The droplets were then cured in a calcium chloride solution. The main objective was to produce mono-sized beads from such a highly viscous and non-Newtonian liquid (1000–5000 mPa s). The effects of nozzle diameter, flow rate and concentration of liquid on the size of the beads were investigated. Among the parameters studied, voltage had a pronounced effect on the size of beads as compared to flow rate, nozzle diameter and concentration of alginate liquid. The size of beads was reduced to a minimum value with increasing the voltage in the range of 0–10 kV. At the early stages of voltage increase (i.e. up to about 4 kV), the rate of size reduction was relatively low, while the dripping mode dominated. However, in the middle part of the range of applied voltage, where the rate of size reduction was high (i.e. about 4–7 kV), an unstable transition occurred between dripping and jetting. At the end part of the range (i.e. 7–10 kV) jet mode of spray was observed. Increasing the height of fall of the droplets was found to improve the sphericity of the beads, because of the increased time of flight for the droplets. This was especially identifiable at higher concentrations of the alginate liquid (i.e. 3 w/v%).展开更多
文摘目的评估自动化磁珠法提取血清脂溶性维生素应用液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测的性能。方法收集200例临床剩余血清样本,采用自动化磁珠法提取血清中脂溶性维生素A,D_(2),D_(3),E和K;同时联合LC-MS/MS检测脂溶性维生素A,D_(2),D_(3),E和K的线性、定量限、精密度、正确度、携带污染率等性能指标以及基质效应。并比较此方法与传统萃取法检测结果的一致性。结果自动化磁珠法提取脂溶性维生素A,D_(2),D_(3),E和K线性相关系数均>0.99;五种物质的定量限分别为5,0.25,0.25,125和0.025ng/ml;批内精密度和批间精密度分别为0.66%~4.83%,0.15%~3.70%;平均加标回收率为87.05%~111.11%;基质效应为95.43%~99.07%;高-低值样本循环进样结果均值与低-低值样本循环进样结果均值之差,均小于低-低值样本循环进样结果均值的3s;统计学结果显示自动化磁珠法和传统萃取法提取的脂溶性维生素结果相关性良好(r>0.99),两种方法的检测结果无显著偏倚。结论自动化磁珠法提取脂溶性维生素的检测性能良好,有望提高样品通量和分析效率。
基金Supported by National Natural Science Foundation of China(81560659&81860771)Science and Technology Project of the Education Department of Jiangxi Province(GJJ201219)+1 种基金Students’Innovative Entrepreneurial Training Plan Program of Jiangxi University of Traditional Chinese Medicine(S202110412003,202010412025,202110412028)Doctoral Research Startup Fund of Jiangxi University of Traditional Chinese Medicine(2018WBZR011)。
文摘[Objectives]To develop a paeonol bead popping gum with hypoglycemic effect.[Methods]The paeonol bead popping gum was prepared by the"two-step method",that is,the pill core was prepared by the guttate pill method,and then the coating was cured by sodium alginate solution and CaCl_(2) solution.The single factor method was used to determine the effects of PEG-4000:paeonol dosage ratio,dropper diameter,condensation time,dropping distance,melting temperature on the comprehensive score of paeonol guttate pill,and the effects of sodium alginate solution concentration,CaCl_(2) solution concentration,number of coating layers,drying time on the comprehensive score of popping gum.Finally,the optimal process was determined and verified by orthogonal experiment method.[Results]When the dosage ratio of PEG-4000:paeonol was 4∶1,the dropper diameter was 4 mm,the condensation time was 5 min,the dropping distance was 6 cm,and the melting temperature was 90℃,the quality of the prepared guttate pill was the optimal.When the concentration of sodium alginate solution was 0.02 g/mL,the concentration of CaCl_(2) solution was 0.25 g/mL,the number of coating layers was 3,and the drying time was 25 min,the appearance and comprehensive score of the obtained popping beads were the optimal.[Conclusions]This study is expected to provide some reference and basis for the development and utilization of hypoglycemic products of traditional Chinese medicine.
文摘Alginate beads, often used for controlled release of enzymes and drugs, are usually produced by spraying sodium alginate liquid into a gelling agent using mechanical vibration nozzle or air jet. In this work an alternative method of electro-spray was employed to form droplets with desired size from a highly viscous sodium alginate solution using constant DC voltage. The droplets were then cured in a calcium chloride solution. The main objective was to produce mono-sized beads from such a highly viscous and non-Newtonian liquid (1000–5000 mPa s). The effects of nozzle diameter, flow rate and concentration of liquid on the size of the beads were investigated. Among the parameters studied, voltage had a pronounced effect on the size of beads as compared to flow rate, nozzle diameter and concentration of alginate liquid. The size of beads was reduced to a minimum value with increasing the voltage in the range of 0–10 kV. At the early stages of voltage increase (i.e. up to about 4 kV), the rate of size reduction was relatively low, while the dripping mode dominated. However, in the middle part of the range of applied voltage, where the rate of size reduction was high (i.e. about 4–7 kV), an unstable transition occurred between dripping and jetting. At the end part of the range (i.e. 7–10 kV) jet mode of spray was observed. Increasing the height of fall of the droplets was found to improve the sphericity of the beads, because of the increased time of flight for the droplets. This was especially identifiable at higher concentrations of the alginate liquid (i.e. 3 w/v%).
