Oil Content Conversion between Ether-based and Ethanol-based Methods and Establishment of Admissible Error for Imported Wool

Due to various reasons, the inspection methods often need to be changed, and the detection reagents often need to be replaced. In this study, a comparative experiment was conducted between the ethanol-based and ether-based determination methods for oil content in imported wool. The determination results obtained from the two methods were treated as abscissa and ordinate respectively,and their linear relationship was analyzed. According to the linear regression analysis, the conversion equation of determination result between the two methods was obtained. In addition, the repeatability admissible error and reproducibility admissible error were established through analyzing the comparative experimental results by scientific software. This study will bring new ideas for further researches in this field, and provide reference for solving the similar problems in actual inspection work.

Chemical Analysis Method for Magnesia and Magnesia-Alumina Refractories——Gravimetric-Molybdenum Blue Photometric Method for Determination of Silicon Dioxide Content

This standard specifies the gravimetric-molybdenum blue photometric method for determination of silicon dioxide content.

Chemical Analysis Method for Carbon Bearing Refractory Products——Determination of Magnesium Oxide Content by CyDTA Volumetric Method

This standard specifies the method summary, reagents, apparatus, sampling, procedure, test results calculation and permissible tolerance of the determination of magnesium oxide by CyDTA volumetric method.

Chemical Analysis of Magnesia and Magnesia-Alumina Refractory Materials——Flame atomic absorption spectrometric method for determination of calcium oxide content

1 Scope This standard specifics the determination of calcium oxide coutent by flame atomic absorption spectrometric method.

A rapid and accurate direct measurement method of underground coal seam gas content based on dynamic diffusion theory

Coal seam gas content is frequently measured in quantity during underground coal mining operation and coalbed methane(CBM)exploration as a significant basic parameter.Due to the calculation error of lost gas and residual gas in the direct method,the efficiency and accuracy of the current methods are not inadequate to the large area multi-point measurement of coal seam gas content.This paper firstly deduces a simplified theoretical dynamic model for calculating lost gas based on gas dynamic diffusion theory.Secondly,the effects of various factors on gas dynamic diffusion from coal particle are experimentally studied.And sampling procedure of representative coal particle is improved.Thirdly,a new estimation method of residual gas content based on excess adsorption and competitive adsorption theory is proposed.The results showed that the maximum error of calculating the losing gas content by using the new simplified model is only 4%.Considering the influence of particle size on gas diffusion law,the particle size of the collected coal sample is below 0.25 mm,which improves the measurement speed and reflects the safety representativeness of the sample.The determination time of gas content reduced from 36 to 3 h/piece.Moreover,the absolute error is 0.15–0.50 m^3/t,and the relative error is within 5%.A new engineering method for determining the coal seam gas content is developed according to the above research.

Study on Colorimetric Method and Content Determination of Total Phenol in Homemade Plum Wine

[Objectives] To study on colorimetric method and content determination of total phenol in homemade plum wine. [Methods]The optimal determination condition of total polyphenols content in plum wine( commercially available and homemade) by Folin-Ciocalteu method was inspected,and commercially available and homemade plum wine was evaluated by the method. [Results]The optimal determination conditions of total polyphenols content: sample dose of 1. 0 m L,Folin-Ciocalteu reagent of 1 m L,4% Na_2CO_3 solution of 4. 0 m L,reaction temperature of 50 ℃,reaction time of 1. 5 h,and determination wavelength of 756 nm. Absorbance showed good linear relationship with total polyphenols content within the range of 17. 73-59. 12 μg/m L( y = 14. 878 x + 0. 0739,R^2= 0. 9998). Recovery rate of adding standard sample was between 98. 8% and 103. 5%,and relative standard deviation was 2. 0%( n = 5). [Conclusions]The method had high precision degree and good stability,which was suitable for measuring total polyphenols content in plum wine( commercially available and homemade).

Technical Study on Extraction of Procyanidins in Lycium ruthenicum Murr. Using Sub-critical Fluid 1,1,1,2-Tetrafluoroethane( R134a)and Content Determination from Different Producing Areas

[Objectives] To study the optimal conditions for extracting procyanidins fromLycium ruthenicum Murr. with sub-critical fluid R134 a( 1,1,1,2-tetrafluoroethane) in 1 L extraction kettle. [Methods]Taking the extraction rate of procyanidins as an indicator,the influence of pressure,temperature,and extraction time on extraction rate of procyanidins fromL. Ruthenicum Murr. was studied by single factor experimental methods and orthogonal array design. [Results]The order of factors affecting extraction rate of procyanidins was extraction temperature > extraction pressure > extraction time. The optimum extraction conditions were as follows: the extraction rate of procyanidins fromL. ruthenicum Murr. was the highest with extraction pressure of 1. 2 MPa,extraction temperature of 50℃ and extraction time of 90 min. The content of procyanidins in L. ruthenicum Murr. from different producing areas was determined by vanillin-HCl method under the optimal conditions. [Conclusions] The method has the advantages of easy operation,good selectivity,low extraction temperature and high extraction efficiency,which is suitable for extraction of procyanidins in L. ruthenicum Murr.

Rapid Determination of Silicon Content in Rice

A method for rapid determination of silicon content in rice was introduced. The reliability of this method was verified by using a recombinant inbred line （RIL） population of rice cross Zhenshan 97B / Milyang 46. Two hundred and forty-nine RILs were transplanted in two replications. Simple correlation coefficients on the silicon content in the hull, flag leaf and stern in rice between duplicate samples of 498 rice materials were 0.97954, 0.97026 and 0.98848, respectively. Ten representative samples were selected for measurement using the high-temperature alkaline fusion method. Simple correlation coefficient between the silicon contents determined by the high-temperature alkaline fusion method and by the present method is 0.9993.

Determination of Bisoprolol Fumarate by Fluorescence Quenching Method

[Objectives]To establish a new method for indirect determination of bisoprolol fumarate based on fluorescence quenching technology.[Methods]In ammonia water and ammonium chloride buffer solution at pH=9.2,whenλexcitation=277 nm andλemission=596 nm,with the increase of CCu2+,the fluorescence signal intensity of bisoprolol fumarate weakened,and the difference between the fluorescence intensity of bisoprolol fumarate itself and the fluorescence intensity of the test solution after the quencher Cu2+was added(ΔF)and Cbisoprolol fumarate showed a good linear relationship.[Results]In the range of 15.39-76.93μg/mL,ΔF=146.7 Cbisoprolol fumarate+482.1,r=0.9988,and the detection limit is 0.1391μg/mL.[Conclusions]The fluorescence quenching method has been applied to the determination of actual samples with a recovery rate of 99.9%and an RSD of 2.7%.The results are satisfactory.

Determination of Active Components of Lamiophlomis rotata(Benth.)Kudo by Ultra-performance Convergence Chromatography

[Objectives]To determine active components of Lamiophlomis rotata(Benth.)Kudo.[Methods]A new method was developed for the quantitative determination of L.rotata by using Ultra-performance convergence chromatography.The separation of active components of L.rotata was successfully achieved on Waters ACQUITY UPC column,with gradient elution carbon dioxide and methanol solvent at flow rate of 0.7 mL/min.The separation gradient elution rate was as follows:15%methanol 0-1 min,18%methanol 1-5 min,20%methanol 5-6 min,25%methanol 6-7 min,30%methanol 7-8 min,30%methanol 8-9 min,15%methanol 9-10 min.The conditions used in the separation process was as follows:column temperature 30℃;injection volume 2μL.Under the abovementioned conditions,the content of methyl glucoside was measured by 3D-full wavelength scanning.The validity of the method was tested by analyzing the precision,reproducibility,stability and accuracy.[Results]The results indicated that in terms of extraction and separation of compounds,supercritical CO2 not only has the diffusion property of gas,but also has the density and fluidity of liquid.[Conclusions]The ultra-high performance chromatography is a new technique for drug analysis.

Physical Properties of the Function and Number of Empirical Macrohardness of the Material: Universal Physical Unit of Measurement of Macro Hardness (Part 2)

Results of analytical studies of the physical properties of the function and number of empirical macrohardness based on the standard experimental force diagram of kinetic macroindentation by a sphere.An analytical comparison method and a criterion for the similarity of the physical and empirical macrohardness of a material are proposed.The physical properties of the hardness measurement process using the Calvert-Johnson method are shown.The physical reasons for the size effect when measuring macrohardness are considered.The universal physical unit and standard of macrohardness of kinetic macroindentation by a sphere is substantiated.

骨骼风痛片的综合质量评价

目的建立测定骨骼风痛片中原薯蓣皂苷等11种成分含量的方法,同时进行化学计量学分析及熵权优劣解距离(EW-TOPSIS)法分析,以综合评价骨骼风痛片的质量。方法采用高效液相色谱法。以Agilent Eclipse Plus C18为色谱柱,以乙腈-0.2%磷酸溶液为流动相进行梯度洗脱,流速为1.0 mL/min,柱温为30℃,检测波长为203 nm(0~28 min,原薯蓣皂苷、甲基原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷)、280 nm(28~60 min,儿茶素、表儿茶素、甘草素、美迪紫檀素、6-姜辣素、8-姜酚、10-姜酚),进样量为10μL。以表儿茶素为内参物,采用一测多评(QAMS)法计算原薯蓣皂苷、甲基原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷、儿茶素、甘草素、美迪紫檀素、6-姜辣素、8-姜酚和10-姜酚的含量,并与外标法检测结果进行比较;采用SPSS 26.0、SIMCA14.1软件进行主成分分析和正交偏最小二乘法-判别分析,以变量重要性投影(VIP)值大于1为标准,筛选影响质量的差异标志物;采用EW-TOPSIS法对15批样品的质量进行综合评价。结果高效液相色谱结合QAMS法测得原薯蓣皂苷、甲基原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷、儿茶素、甘草素、美迪紫檀素、6-姜辣素、8-姜酚和10-姜酚的含量分别为6.330~10.863、1.150~2.274、0.431~0.740、2.818~4.823、0.826~1.510、0.043~0.094、0.079~0.231、0.479~1.020、0.146~0.288、0.118~0.318 mg/g,与外标法比较差异均无统计学意义(P>0.05);15批样品可分为3组,S1~S6、S7~S10、S11~S15分别聚为一组;原薯蓣皂苷、表儿茶素、薯蓣皂苷、6-姜辣素的VIP值均大于1;15批样品的最优解欧氏贴近度(Ci)为0.1635~0.7037,其中S11~S15样品的Ci值均大于0.6。结论所建QAMS法准确、简便,结合化学计量学分析及EW-TOPSIS法可用于综合评价骨骼风痛片的质量;原薯蓣皂苷、表儿茶素、薯蓣皂苷和6-姜辣素可能是影响骨骼风痛片质量的差异标志物;S11~S15样品的质量较好。

不同干燥方式对茯苓药材中三萜类及茯苓酸含量的影响

采用不同干燥方式(自然晒干、60℃烘干、80℃烘干、105℃烘干、冻干)对茯苓(Poria cocos)鲜品进行干燥,测定干燥后的茯苓三萜类及茯苓酸含量,比较不同干燥方式对其三萜类及茯苓酸含量的影响。结果表明,茯苓三萜类及茯苓酸含量均为冻干>105℃烘干>80℃烘干>60℃烘干>自然晒干,冻干工艺下茯苓三萜及茯苓酸含量分别高达8.95%、6.89%,自然晒干下的茯苓三萜类及茯苓酸含量均最低。确定了茯苓药材的最佳干燥方式,为茯苓药材后期加工工艺的选用提供参考。

响应面法优化肉桂子总有机酸提取工艺及其抗氧化活性研究

采用响应面法优化肉桂子中总有机酸的提取工艺并研究其体外抗氧化活性。根据Box-Behnken Design设计原理,分别考察乙醇浓度、料液比、超声功率、超声时长对肉桂子总有机酸得率的影响。以肉桂子总有机酸得率为响应值,通过响应面法确定肉桂子总有机酸的最佳提取工艺。采用DPPH法、铁离子还原能力评价肉桂子总有机酸抗氧化能力。结果表明,单因素影响顺序依次为料液比>乙醇浓度>超声时长。肉桂子中总有机酸的最优提取工艺为:乙醇浓度59%、料液比1:60(g/mL)、超声功率350 W,超声时长49 min,得到的总有机酸的平均得率9.77%。VC及S-1肉桂子的IC50分别为0.01119、0.01437 mg/mL。说明该提取工艺稳定、可行、可靠;肉桂子具有一定抗氧化能力。

甘薯抗性淀粉研究进展

甘薯是重要的淀粉作物,其块根中抗性淀粉(RS)含量较高,具备良好的产品开发潜力。要进一步促进甘薯RS的应用和推广,不仅需要筛选或培育出RS含量更高的甘薯品种,还需要加大开发甘薯深加工淀粉产品。除调控淀粉合成相关基因的表达外,生产实际中还可通过调整栽培措施等方式提高甘薯RS的含量。通过化学修饰法、物理法和酶解法等方法可制备甘薯RS产品,也能提高产品中RS的含量。本文系统综述了近年来甘薯淀粉的保健效果、RS含量的测定方法、影响甘薯淀粉中RS含量的因素、RS的制备方法及其特性等方面的进展,为未来甘薯中RS的制备、产量提高、产品开发和推广提供参考。

动物性饲料原料中铁元素含量的快速检测方法研究

研究旨在建立一种利用分光光度法快速检测动物性饲料原料中铁元素含量的方法。采用两种分光光度法(邻菲罗啉法和硫氰酸钾法)对动物性饲料原料灰分中铁元素进行检测。结果显示:试验确定原料中铁元素以Fe^(3+)形式存在,选择硫氰酸钾法作为后续试验的检测方法,优化后硫氰酸钾法的最适条件为:灰化时间3.5 h、检测波长480 nm、硫氰酸钾溶液体积1.0 mL、显色时间10 min、显色反应温度30℃,显色反应过程无须避光。在此参数下测定得到标准曲线在1~20 mg/L范围内具有良好线性关系(R2>0.999 0),方程为y=0.071 5x+0.009(R^(2)=0.999 4)。硫氰酸钾法的稳定性好、准确度高、抗干扰性强,批次内相对标准偏差为1.03%~2.05%,6批次鸡肉粉样品加标回收率为98.02%~101.03%,10~50倍Fe^(3+)浓度的Na^(+)、K^(+)和Ca^(2+)不会干扰Fe^(3+)含量的检测,具有替代原子吸收光谱法进行快速检测的可行性。使用两个方法同时测定11种动物性原料样品中铁元素含量的结果差异不显著(P>0.05)。研究表明,试验建立的硫氰酸钾法可用于宠物食品动物性饲料原料中铁元素含量的快速检测。

发酵液中乳酸含量测定方法比较研究

为寻找高效便捷、成本低廉的乳酸测定方法,对比研究了三氯化铁法和对羟基联苯法对尾菜发酵液中乳酸含量的测定性能。结果显示,三氯化铁法和对羟基联苯法的线性方程相关系数均大于0.99,检出限分别为9.70×10^(-2)g/L和2.35×10^(-3)g/L,均满足分析测试要求;精密度测定中,三氯化铁法和对羟基联苯法的相对标准偏差(RSD)分别为1.19%~3.53%和2.54%~3.71%,加标回收率分别为99.3%~105.2%和102.7%~109.1%;杂质的存在对三氯化铁法的测定结果影响较小,但对对羟基联苯法的测定结果有较大影响;统计学检验表明,两种方法对发酵液中乳酸含量的测定结果无显著性差异;与对羟基联苯法相比,三氯化铁法操作简便,测定速度快,试剂成本低,所需样品量少,是较为优异的乳酸含量测定方法,具有广阔的应用前景。

HPLC-UV法测定舒肝和胃丸中α-香附酮和香附烯酮的含量

目的:建立舒肝和胃丸中α-香附酮和香附烯酮的高效液相色谱(HPLC-UV)含量测定法,为该制剂中醋香附含量的质量控制提供依据。方法:对舒肝和胃丸中α-香附酮和香附烯酮同时进行含量测定。采用Agilent ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相为甲醇和水(65∶35),流速1.0 mL·min^(-1),检测波长254 nm,柱温30℃,进样量5μL。结果:采用该方法得到的舒肝和胃丸色谱图中,α-香附酮和香附烯酮色谱峰与相邻色谱峰分离效果较好,满足含量测定的要求;指标性成分α-香附酮、香附烯酮分别在0.08036~0.80360μg、0.2112~2.1120μg范围内线性关系良好,相关系数均为1.000;平均加标回收率分别为102.0%(RSD:1.6%,n=6),102.4%(RSD:2.0%,n=6);稳定性(24 h)、重复性、精密度良好。结论:本研究建立的α-香附酮和香附烯酮HPLC-UV含量测定方法简单、快捷、准确,可为舒肝和胃丸中醋香附含量的控制提供依据。

抗血小板药物的质量研究进展

抗血小板药物近年来呈现蓬勃发展的态势,其质量控制标准也在不断发展和完善。本综述基于《中华人民共和国药典》2020年版(ChP 2020)、《美国药典》43版(USP 43)、《日本药典》17版(JP 17)等国内外及相关指导原则等参考资料,全面归纳了抗血小板药物在药典中的收录情况,对常见的抗血小板药物的质量控制方法进行总结,对含量测定和体内药物分析方法等项目进行全面分析,期望为抗血小板药物的研究与开发提供参考。

益母草当归锭的制备及主成分阿魏酸含量测定

为确定益母草当归锭的制备工艺,并制定益母草当归锭主要成分阿魏酸的含量限度,本试验以益母草和当归为原料,将其超微粉碎后得到微粉,加入黏合剂,通过湿法制粒得到软材,再经过制粒、整粒、压片等步骤,制得益母草当归锭;采用高效液相色谱法对阿魏酸含量检测方法的专属性、线性、重复性、精密度、耐受性以及加样回收试验等方法学进行考察,并通过对制备的10批样品进行检测,建立益母草当归锭中阿魏酸的含量检测方法及限度。结果显示,制得的益母草当归锭为表面光滑的圆柱状,每锭质量达120 g;阿魏酸的高效液相色谱检测方法专属性、线性、重复性、精密度、耐受性以及加样回收试验结果均良好;测得10批样品中阿魏酸的含量为0.34~0.52 mg/g,考虑到当归药材的产地、来源、炮制加工、生产及贮存等因素对阿魏酸含量的影响,将阿魏酸含量限度在最小值的基础上下降10%,暂定阿魏酸含量不得少于0.31 mg/g,作为益母草当归锭的含量检测限度。结果表明,本试验益母草当归锭制备方法简单,每锭载药量大,1锭即可达到治疗剂量,方便投喂,建立的阿魏酸高效液相色谱含量检测方法稳定、可行,可用于益母草当归锭的质量控制。