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保泰松糖衣片溶出度测定方法改进研究

沈阳药科大学学报 2022年第2期39卷 156-163页

作者：王柳孙婷王琛赵春杰姜建国乔晓宁蒋凝沈阳药科大学药学院辽宁沈阳110016 河北省药品医疗器械检验研究院河北石家庄050011

目的改进保泰松糖衣片的溶出度测定方法。方法采用七种溶出介质和三个不同转速对保泰松溶出方法进行考察,对比不同厂家样品的溶出行为。应用高效液相色谱法测定保泰松溶出量,色谱柱为Agilent Eclipse XDB-C_(18)(250 mm×4.6 mm,5μm),... 详细信息

目的改进保泰松糖衣片的溶出度测定方法。方法采用七种溶出介质和三个不同转速对保泰松溶出方法进行考察,对比不同厂家样品的溶出行为。应用高效液相色谱法测定保泰松溶出量,色谱柱为Agilent Eclipse XDB-C_(18)(250 mm×4.6 mm,5μm),柱温30℃,以0.02 mol·L^(-1)醋酸钠缓冲液-乙腈(体积比30∶70,V/V)为流动相,检测波长为240 nm,流速1.0 mL·min^(-1),进样量20μL。结果确立以磷酸盐缓冲液(pH6.8)900 mL为溶出介质,转速为100 r·min^(-1)的溶出条件,不同厂家保泰松片的溶出曲线存在明显差异。保泰松在0.01~0.40 g·L^(-1)质量浓度内线性关系良好(r=0.9999),室温放置8 h稳定。结论该溶出方法区分力效果好,可行性强,测定方法较原紫外分光光度法灵敏度更高、准确度更好,可为提高保泰松片的质量标准,建立合理的溶出度测定方法提供技术支持。

关键词：高效液相色谱法保泰松溶出度溶出曲线紫外-分光光度法方法改进

反相高效液相色谱法测定尼尔雌醇原料及片剂的有关物质和含量

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中国药业 2019年第5期28卷 33-36页

作者：孙婷张菁刘云姜建国王柳乔晓宁河北省药品检验研究院河北石家庄050011 河北省石家庄市食品药品检验中心河北石家庄050011

目的建立测定尼尔雌醇原料及片剂的有关物质和含量的反相高效液相色谱(RP-HPLC)法。方法色谱柱为Waters Symmetry C18柱(250 mm×4. 6 mm,5μm),流动相为0. 02 mol/L乙酸铵溶液-乙腈(40∶60,V/V)等度洗脱,流速为1. 0 m L/min,柱温为35℃... 详细信息

目的建立测定尼尔雌醇原料及片剂的有关物质和含量的反相高效液相色谱(RP-HPLC)法。方法色谱柱为Waters Symmetry C18柱(250 mm×4. 6 mm,5μm),流动相为0. 02 mol/L乙酸铵溶液-乙腈(40∶60,V/V)等度洗脱,流速为1. 0 m L/min,柱温为35℃,检测波长为280 nm,进样量为20μL。结果尼尔雌醇峰和相邻杂质峰均能达到完全有效分离;尼尔雌醇质量浓度在0. 01~2. 0 g/L范围内与峰面积线性关系良好;平均回收率为100. 00%,RSD为1. 29%(n=9)。1批原料和3批片剂样品含量测定结果分别为99. 79%,98. 62%,98. 71%,98. 56%,单个最大杂质分别为0. 14%,0. 41%,0. 39%,0. 40%,总杂质分别为0. 49%,0. 78%,0. 76%,0. 75%。结论建立的RP-HPLC法能有效测定尼尔雌醇原料及片剂的有关物质和含量,为该类药物工艺过程控制、监管和质量保障提供了一定的技术支持。

关键词：口服雌激素类药物尼尔雌醇尼尔雌醇片有关物质含量测定反相高效液相色谱法

NIR assignment of isopsoralen by 2D-COS technology and model application in Yunkang Oral Liquid

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Journal of Innovative Optical Health Sciences 2015年第6期8卷 1-8页

作者： Yanling Pei Zhisheng Wu Xinyuan Shi xiaoning Pan Yanfang Peng Yanjiang qiao Beijing University of Chinese Medicine Beijing 100102 P.R.China Beijing Key Laboratory for Basic and Development Research on Chinese Medicine Beijing 100102P.R.China Key Laboratory of TCM-Information Engineer of State Administration of TCM Beijing 100102 P.R.China

Near infrared(NIR)assignment of Isopsoralen was performed using deuterated chloroform solvent and two-dimensional correlation spectroscopy(2D-COS)*** Oral Liquid was applied to study Isopsoralen,the characteristic bands by spectral assignment as well as the bands by interval partial least squares(iPLS)and synergy interval partial least squares(siPLS)were used to establish partial least squares(PLS)*** coefficient of determination in calibration(R^(2)_(cal))were 0.9987,0.9970 and *** coefficient of determination in cross validation(R^(2)_(val)) T were 0.9985,0.9921 and *** coe±cient of determination in prediction(R^(2)_(pre)) T were 0.9987,0.9955 and *** root mean square error of calibration(RMSEC)were 0.27,0.40 and 0.31 *** root mean square error of cross validation(RMSECV)were 0.30,0.67 and 0.32 *** root mean square error of prediction(RMSEP)were 0.23,0.43 and 0.22 *** residual predictive deviation(RPD)were 31.00,16.58 and *** turned out that the characteristic bands by spectral assignment had the same results with the chemometrics methods in PLS *** provided guidance for NIR spectral assignment of chemical compositions in Chinese Materia Medica(CMM).

关键词： Near infrared spectroscopy two-dimensional correlation spectroscopy Isopsoralen Yunkang Oral Liquid spectral assignment

高效液相色谱法同时测定盐酸拉贝洛尔片中的3种杂质

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化学分析计量 2022年第11期31卷 27-31页

作者：郝丽娟徐艳梅乔晓宁闫凯盖成高燕霞河北省药品医疗器械检验研究院国家药品监督管理局仿制药质量控制与评价重点实验室石家庄050227

建立高效液相色谱(HPLC)法同时测定盐酸拉贝洛尔片中2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸、2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸甲酯和2-羟基-5-(2-(4-苯基丁-2-氨基)乙酰)苯甲酰胺的含量。采用... 详细信息

建立高效液相色谱(HPLC)法同时测定盐酸拉贝洛尔片中2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸、2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸甲酯和2-羟基-5-(2-(4-苯基丁-2-氨基)乙酰)苯甲酰胺的含量。采用以十八烷基硅烷键合硅胶为填料的Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm)分离,以体积分数为0.1%的磷酸溶液为流动相A,乙腈–体积分数为0.1%的磷酸溶液(体积比为50∶50)为流动相B,流量为1.5 mL/min,梯度洗脱,检测波长为230 nm,柱温为40℃,进样体积为20μL。盐酸拉贝洛尔与3种杂质及强降解物之间均分离良好,3种杂质的质量浓度与其色谱峰面积具有良好的线性关系,相关系数均为0.9999,检出限为0.151~0.154 ng/mL。3种杂质测定值的相对标准偏差均小于2%(n=6),平均加标回收率为98.0%~98.9%。该方法简便、快速,可用于同时测定盐酸拉贝洛尔片中3种杂质,以便更好地控制盐酸拉贝洛尔片的质量。

关键词：高效液相色谱法盐酸拉贝洛尔片有关物质 2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸 2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸甲酯 2-羟基-5-(2-(4-苯基丁-2-氨基)乙酰)苯甲酰胺

Sensitive detection of thyroid stimulating hormone by inkjet printed microchip with a double signal amplification strategy

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Chinese Chemical Letters 2018年第12期29卷 1879-1882页

作者： Beibei Yang Dongmei Liu Lina Zhu Yun Liu xiaoning Wang Liang qiao Weijia Zhang Baohong Liu Department of Chemistry Shanghai Stomatological HospitalCollaborative Innovation Center of Chemistry for Energy MaterialsFudan UniversityShanghai 200433China Department of Pharmacy Qingdao Municipal HospitalQingdao 266001China

An electrochemical immunosensor for sensitive detection of thyroid stimulating hormone(TSH) has been developed by using an inkjet printed microchip and based on a double signal amplification strategy using magnetic beads(MBs), alkaline phosphatase(ALP) and p-aminophenyl phosphate(pAPP) *** pulse voltammetry(DPV), cyclic voltammogram(CV) and amperometric i-t curve(i-t) were employed to characterize the immunosensor. High sensitivity and good selectivity were observed. The detection linear range was from 0.01 μIU/mL to 10 μIU/mL, in which the peak currents increased along with the concentration. The detection limit was 0.005 μIU/mL at S/N = 3. The immunosensor was also applied for TSH detection in human serum with recoveries from 98.0% to 101.8% and relative standard deviations from 1.3% to 3.1%, demonstrating potential value in clinical diagnosis.

关键词： Electrochemical immunosensor Inkjet printed microchip Signal amplification Thyroid stimulating hormone Alkaline phosphatase

The Impact of Varied Fertilizers on the Yield and Quality of Panicum miliaceum under Low Nitrogen Conditions

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Phyton-International Journal of Experimental Botany 2024年第10期93卷 2629-2644页

作者： Mengyao Wang Jiao Mao Yuanmeng Xu Shu Wang Yuhan Liu Jiangling Ren Sichen Liu Zhijun qiao xiaoning Cao Center for Agricultural Genetic Resources Research Shanxi Agricultural UniversityTaiyuan030031China College of Agriculture Shanxi Agricultural UniversityJinzhong030801China Key Laboratory of Crop Genetic Resources and Germplasm Development in Loess Plateau Ministry of Agriculture and Rural AffairsTaiyuan030031China

To clarify the response characteristics of broomcorn millet yield and quality to various fertilizers under low nitrogen conditions,the present study investigated the effects of different fertilization treatments,including no fertilization(HCK,CCK),urea(HF1,CF1),phosphate fertilizer(HF2,CF2),compound fertilizer(HF3,CF3),and organic fertilizer(HF4,CF4),on the agronomic traits,quality,and starch pasting properties of proso *** experimental materials,non-waxy proso millet(Hequ red proso millet,denoted as HQH)and waxy proso millet(Chishu 1,denoted as CS1)were *** results showed that under low nitrogen conditions,urea treatment(HF1)significantly increased plant height and yield,and phosphate fertilizer treatment(HF2)significantly increased thousand-grain weight(TW).For waxy proso millet Chishu NO.1(CS1),urea treatment(CF1)significantly increased yield,phosphate fertilizer treatment(CF2)significantly influenced the height of the plants,and compound fertilizer treatment(CF3)significantly increased thousand-grain *** terms of quality,phosphate fertilizer treatment(CF2)and organic fertilizer treatment(CF4)resulted in a substantial augmentation of both the total starch content and amylose content of waxy proso millet Chishu NO.1(CS1),respectively,and organic fertilizer treatment(HF4,CF4)resulted in a notable enhancement of the protein content of proso *** fertilizer treatment(HF4)increased peak viscosity(PV),hot viscosity(HV),setback viscosity(SV),final viscosity(FV),breakdown viscosity(BV),pasting time(PTim),and pasting temperature(PTemp)of non-waxy proso *** fertilizer treatment(CF2)increased the peak viscosity(PV),hot viscosity(HV),breakdown viscosity(BV),final viscosity(FV),pasting time(PTim),and pasting temperature(PTemp)of waxy proso *** fertilizer treatment(HF4)and phosphate fertilizer treatment(CF2)under low nitrogen were the most effective in improving the comprehensive quality of non-waxy and waxy proso millet,r

关键词： Proso millet low nitrogen yield quality

高效液相色谱-质谱联用法同时测定盐酸二甲双胍肠溶片中6种亚硝胺类基因毒性杂质

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化学分析计量 2022年第5期31卷 28-32页

作者：徐艳梅李挥张素平乔晓宁苗会娟盖成王茉莉高燕霞河北省药品医疗器械检验研究院石家庄050200

建立高效液相色谱–质谱联用法同时测定盐酸二甲双胍肠溶片中6种N-亚硝胺类基因毒性杂质(N-亚硝基二甲胺、N-亚硝基-N-甲基-4-氨基丁酸、N-亚硝基二乙胺、N-亚硝基乙基异丙胺、N-亚硝基二异丙胺和N-亚硝基二丁胺)。采用ACE C_(18)柱(150... 详细信息

建立高效液相色谱–质谱联用法同时测定盐酸二甲双胍肠溶片中6种N-亚硝胺类基因毒性杂质(N-亚硝基二甲胺、N-亚硝基-N-甲基-4-氨基丁酸、N-亚硝基二乙胺、N-亚硝基乙基异丙胺、N-亚硝基二异丙胺和N-亚硝基二丁胺)。采用ACE C_(18)柱(150 mm×4.6 mm,5μm),流动相为0.1%甲酸水–甲醇,流量为0.6 mL/min,梯度洗脱,柱温为40℃,采用正离子多反应监测(MRM)模式,以大气压化学电离源为离子源。6种N-亚硝胺类基因毒性杂质的质量浓度在各自的线性范围内与色谱峰面积线性关系良好,相关系数均不小于0.9995。检出限和定量限分别为0.0337~0.03389 ng/mL和0.10076~0.10268 ng/mL。样品平均加标回收率为97.83%~103.33%,测定结果的相对标准偏差为1.19%~4.45%(n=9)。该方法专属性强,简单、快速、灵敏,适用于测定盐酸二甲双胍肠溶片中的N-亚硝胺类基因毒性杂质。

关键词：液相色谱-质谱法盐酸二甲双胍肠溶片基因毒性杂质

Pulse electrochemical synaptic transistor for supersensitive and ultrafast biosensors

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InfoMat 2023年第11期5卷 25-39页

作者： Jianlong Ji Zhenxing Wang Fan Zhang Bin Wang Yan Niu xiaoning Jiang Zeng-ying qiao Tian-ling Ren Wendong Zhang Shengbo Sang Zhengdong Cheng Qijun Sun College of Electronics Information and Optical Engineering Taiyuan University of TechnologyTaiyuanthe People’s Republic of China Beijing Institute of Nanoenergy and Nanosystems Chinese Academy of SciencesBeijingthe People’s Republic of China Department of Mechanical and Aerospace Engineering North Carolina State UniversityRaleighNorth CarolinaUSA D Artificial Intelligence Biomedical Research Institute Taiyuanthe People’s Republic of China CAS Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety CAS Center for Excellence in NanoscienceNational Center for Nanoscience and Technology(NCNST)Beijingthe People’s Republic of China Institute of Microelectronics Tsinghua UniversityBeijingthe People’s Republic of China College of Chemical and Biological Engineering Zhejiang UniversityHangzhouthe People’s Republic of China

High sensitivity and fast response are the figures of merit for benchmarking commercial *** to the advantages of intrinsic signal amplification,bionic ability,and mechanical flexibility,electrochemical transistors(ECTs)have recently gained increasing popularity in constructing various *** the current work,we have proposed a pulse-driven synaptic ECT for supersensitive and ultrafast *** pulsing the presynaptic input(drain bias,VD)and setting the modulation potential(gate bias)near transconductance intersection(VG,i),the synaptic ECT-based pH sensor can achieve a record high sensitivity up to 124 mV pH^(-1)(almost twice the Nernstian limit,59.2 mV pH^(-1))and an ultrafast response time as low as 8.75 ms(7169 times faster than the potentiostatic sensors,62.73 s).The proposed synaptic sensing strategy can effectively eliminate the transconductance fluctuation issue during the calibration process of the pH sensor and significantly reduce power ***,the most sensitive working point at VG,i has been elaborately figured out through a series of detailed mathematical derivations,which is of great significance to provide higher sensitivity with quasi-nonfluctuating amplification *** proposed electrochemical synaptic transistor paired with an optimized operating gate offers a new paradigm for standardizing and commercializing high-performance biosensors.

关键词： fast response pH sensor pulse electrochemical transistor supersensitive synaptic transistor

采用通量线-有限元混合方法求解有风条件下直流输电线路离子流场

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电工技术学报 2019年第5期34卷 910-916页

作者：乔骥葛小宁邹军电网环境保护国家重点实验室武汉430074 电力系统及发电设备控制和仿真国家重点实验室(清华大学电机系) 北京100084

直流输电线路电晕产生的空间电荷在直流电场力的作用下形成离子流,会显著增强地面电场强度。结合通量线法和有限元法各自的特点,提出一种混合方法求解离子流场,在分裂导线周围的区域采用通量线法,在远离导线的区域采用有限元法,各区域... 详细信息

直流输电线路电晕产生的空间电荷在直流电场力的作用下形成离子流,会显著增强地面电场强度。结合通量线法和有限元法各自的特点,提出一种混合方法求解离子流场,在分裂导线周围的区域采用通量线法,在远离导线的区域采用有限元法,各区域之间采用D-N交替法进行耦合计算。一方面,仅在导线周围采用通量线法,避免了通量线法在全空间由于Deutsch假设产生的误差,并且可以考虑风速影响;另一方面,分裂导线周围不需要网格剖分,能够有效减少有限元网格节点数量,提高有限元计算效率。同时通量线法能够为有限元法提供交界面的初始值,耦合迭代在较少步数内即可收敛。计算结果与实验结果吻合较好,求解效率得到提高。最后,采用该方法对±800 kV与±500 kV直流同塔双回线路地面电场强度与离子流密度进行了预测分析。

关键词：离子流直流输电线路通量线法上流有限元法区域分解法