HPLC-PAD法同时测定维药祖卡木颗粒中甘草苷、柚皮苷、槲皮素和山奈酚的含量

建立采用超声提取、高效液相色谱-二极管阵列检测法测定祖卡木颗粒中甘草苷、柚皮苷、槲皮素和山奈酚含量的方法。色谱柱:安捷伦HC-C18柱(250 mm×4.6 mm,5μm);流动相:乙腈(A)-0.1%磷酸溶液(B),梯度洗脱;检测波长286 nm,365 nm,柱温30℃,流速1.0 m L/min。结果表明,甘草苷、柚皮苷、槲皮素和山奈酚分别在0.2⁴0μg/m L(r=0.999 8)和1.040μg/m L(r=0.999 8)和1.0⁶0μg/m L(r=0.999 9),0.560μg/m L(r=0.999 9),0.5⁶0μg/m L(r=0.999 9)和0.560μg/m L(r=0.999 9)和0.5⁶0μg/m L(r=0.999 8)浓度范围内呈良好的线性关系,平均回收率分别为102.8%(RSD=1.08%,n=5),97.3%(RSD=0.65%,n=5),103.6%(RSD=1.36%,n=5)和101.4%(RSD=1.63%,n=5)。该方法简便、快速、有效、灵敏、准确、具有良好的重复性和回收率,可作为该药物的定量分析方法。     

UPLC法同时测定蒲黄中两种黄酮类成分

采用超高效液相色谱法测定蒲黄水提液中香蒲新苷和异鼠李素-3-O-新橙皮糖苷的含量。采用UPLC,色谱柱:ACQUITY UPLC~? HSS T3(1. 8μm,2. 1 mm×100 mm),波长:254 nm、柱温:30℃、进样量:1. 4μL、以0. 3 m L/min乙腈-0. 1%甲酸溶液梯度洗脱。香蒲新苷的线性范围为0. 09369～0. 468μg,r=0. 9996(n=6),回收率为104. 76%,RSD=2. 16%(n=6);异鼠李素-3-O-新橙皮糖苷线性范围为0. 1441～0. 72072μg,r=0. 9996(n=6);回收率为103. 31%,RSD=2. 37%(n=6)。表明该方法操作简便,重复性好,结果准确,可用于蒲黄中两种黄酮类成分的含量测定。     

高效液相色谱法测定2,4-二苯基-1,5-苯并硫氮杂-α-(丁二酰亚胺基)-β-内酰胺

建立了测定 2 ,4 -二苯基 - 1,5 -苯并硫氮杂 -α- (丁二酰亚胺基 ) -β-内酰胺高效液相色谱法。该法线性范围在 0～0 .1m g/ m L ,回归方程为 A=196 7346 75 .7c- 35 84 32 .3,相关系数 r=0 .9993,相对标准偏差 0 .38% (c=0 .0 6 mg/ m L ,n=5 ) ,检出限为 0 .0 6μg/ m L。平均回收率在 95 .7%～ 10 3.9%之间     

高效液相色谱法测定盐酸二甲双胍片含量的优化

目的:优化高效液相色谱法测定盐酸二甲双胍片含量。方法:采用Waters Symmerty~? C18(250 mm×4.6 mm,5μm)色谱柱,以0.005 mol/L磷酸二氢钠与0.01mol/L戊烷磺酸钠混合溶液(磷酸调节pH值3.0)-乙腈(94∶6)为流动相,柱温30℃,流速1.0mL/min,进样量5μL,检测波长233nm。结果:盐酸二甲双胍质量浓度在140.36～421.08μg/mL范围内,线性关系良好(r=1.0000),平均回收率为99.10%,RSD为0.54%(n=9)。结论:本方法简便、快速、准确,可用于盐酸二甲双胍片含量的测定。     

HPLC法测定铁甲草中大黄素的含量

建立铁甲草中大黄素的含量测定方法。采用高效液相色谱法(HPLC)测定铁甲草中大黄素的含量,应用Waters XBridgePeptide BEH C18(4. 6 mm×250 mm,5μm)色谱柱,以甲醇-0. 1%甲酸(85∶15)为流动相,流速1. 0 m L/min,柱温35℃,进样量为10μL,检测波长254 nm,测定大黄素的含量。大黄素浓度在5～50μg/m L范围内呈良好线性关系(Y=38315X-16555,R2=0. 9994),平均回收率为98. 94%,RSD为1. 98%(n=6)。本文方法准确灵敏、稳定可靠,可用于铁甲草中大黄素的含量测定。     

反相悬浮法合成高吸水性树脂的研究

以过硫酸钾为引发剂 ,N ,N 亚甲基双丙烯酰胺为交联剂 ,采用反相悬浮法合成了聚丙烯酸钠高吸水性树脂。反应最佳原料配比为 :单体中和度 80 % ,m (引发剂 )∶m(单体 ) =0 .1∶10 0 ,m(交联剂 )∶m(单体 ) =0 0 5∶10 0 ,m(油相 )∶m(水相 ) =2 2∶1 0 ,在此条件下产品的吸水率 (6 6 0g/g)和吸盐水率 (6 4g/g)最高 ,吸盐水速度较快 (2 9 6s) ,热稳定性良好 ,在 2 5 0℃以下热处理对其吸水性能无明显影响。引入非离子性单体聚丙烯酰胺AM ,使n (AM)∶n (AA +AM) =0 3∶1 0 ,能显著提高产物的吸水速度 (3s)和吸盐水率 (>10 0g/g)。水中金属离子和有机溶剂的存在使产物的吸水率显著降低     

高效液相色谱法同时测定尼卡巴嗪中4,4'-二硝基均苯二脲和2-羟基-4,6-二甲基嘧啶的含量

建立了同时测定尼卡巴嗪中4,4'-二硝基均苯二脲(DNC)和2-羟基-4,6-二甲基嘧啶(HDP)双组分的高效液相色谱法。实验采用安捷伦Poroshell 120 Bonus-RP色谱柱(4. 6 mm×150 mm,2. 7μm),水和乙腈为流动相梯度洗脱,流速为0. 8 m L/min,柱温为40℃,HDP和DNC的检测波长均选择300 nm。试验结果表明HDP和DNC分别在23. 3～34. 9μg/m L和56. 7～85. 1μg/m L范围内线性关系良好,相关系数(r)分别为0. 999 8和0. 999 6。HDP平均回收率为100. 4%,RSD为0. 9%(n=9); DNC的平均回收率为99. 2%,RSD为0. 8%(n=9)。建立的方法简便、准确、可靠,可更好地控制尼卡巴嗪的质量。     

反相液相色谱法测定7-羟基-3,4-二氢-2(1H)-喹啉酮的含量

建立了反相液相色谱测定7-羟基-3,4-二氢-2(1H)-喹啉酮含量的方法。采用shim-pack C18柱(5μm,4.6mmi.d.×250mm),流动相为v(甲醇)∶v[缓冲溶液(含事先配制好的0.075mol/L的磷酸二氢铵,磷酸调至pH=3)]=50∶50,流速为0.8mL/min,检测波长为250nm。外标法定量,7-羟基-3,4-二氢-2(1H)-喹啉酮1～100μg/mL浓度范围内呈良好的线性关系,线性回归系数r为0.9997,平均回收率为99.26%,RSD=1.17%(n=9)。     

HPLC法测定复方利血平片中氢氯噻嗪、硫酸双肼屈嗪、维生素B1和维生素B6的含量

采用HPLC法测定复方利血平片中氢氯噻嗪、硫酸双肼屈嗪、维生素B1和维生素B6的含量。Kromasil C-18色谱柱(250 mm×4.6 mm,5μm),检测波长210 nm,以0.2%己烷磺酸钠(用冰醋酸调节pH=3.5)-甲醇-乙腈(75∶20∶5)为流动相,流速1.0 mL/min,进样量20μL,柱温30℃。结果表明,氢氯噻嗪的线性范围为49.6～496.0μg/mL(R2=0.999 4),精密度RSD为0.12%(n=6),重复性RSD为0.45%(n=6),平均回收率为99.74%(RSD=0.78%,n=9);硫酸双肼屈嗪的线性范围为16.8～336.0μg/mL(R2=0.999 3),精密度RSD为0.06%(n=6),重复性RSD为0.21%(n=6),平均回收率为99.83%(RSD=0.08%,n=9);维生素B1的线性范围为4.0～80.0μg/mL(R2=0.998 7),精密度RSD为0.56%(n=6),重复性RSD为0.96%(n=6),平均回收率为99.02%(RSD=1.13%,n=9);维生素B6的线性范围为4.0～80.0μg/mL(R2=0.999 1),精密度RSD为0.23%(n=6),重复性RSD为0.78%(n=6),平均回收率为99.56%(RSD=0.48%,n=9)。此法分离度好,峰形对称,分析周期短,重复性好,简单易行,可同时测定复方利血平片中氢氯噻嗪、硫酸双肼屈嗪、维生素B1和维生素B6的含量。     

HPLC法测定广西野生酸荔枝核中β-谷甾醇含量

建立测定广西野生酸荔枝核中β-谷甾醇含量的方法。采用C18-Inertsil-ODS-3(4. 6 nm×250 nm,5μm),以乙腈-甲醇-异丙醇(90∶9∶1)为流动相,流速1. 0 m L/min,柱温25℃,检测波长为205 nm。回归方程为Y=-0. 30767+10. 70741X,β-谷甾醇在7. 28～36. 4μg/m L范围内和峰面积呈良好线性关系,线性相关系数为0. 9999。稳定性实验测定了0～8 h(n=5)测得酸荔枝核提取物中β-谷甾醇含量的是0. 01843%,RSD小于1%。本方法简便可靠,重复性和定性好,可对广西野生酸荔枝核提取物中β-谷甾醇含量进行测定。     

蜂巢石对水中正磷酸盐的吸附性能

该文研究了不同初始浓度、温度和振荡时间条件下蜂巢石矿物质对水中正磷酸盐的吸附行为。结果表明在蜂巢石投加量不变的情况下,蜂巢石对低浓度正磷酸盐有较强的吸附能力,平均吸附率达45％;蜂巢石对正磷酸盐的吸附在10min时达到最大吸附量,体现了快速吸附的特点;该反应是吸热反应,蜂巢石对正磷酸盐的去除率随着温度的升高而增加;正磷酸盐在蜂巢石中易于脱附,2h内的脱附量可达93％;蜂巢石对正磷酸盐的吸附行为符合Langmuir和Freundlich吸附等温式拟合,吼值和1／n值表现为优先吸附,且其吸附兼有物理吸附及化学吸附两种作用。     

镁离子对水溶性聚磷酸铵的水解影响研究

近年来水溶性聚磷酸铵（APP）作为螯合液体肥在农业上得到了广泛关注和应用。以两种不同聚合度分布的水溶性APP为原料,系统研究了Mg²⁺对两种水溶性APP的水解的影响。研究结果表明：在60 ℃反应110 h后,APP2溶液中Mg²⁺的质量分数为0、0.5%、1.0%、1.5%、2.0%时,其正磷酸铵的质量分数从未反应时的8.1%分别变为32.7%、31.3%、28.1%、30.7%、32.1%;APP8溶液中Mg²⁺的质量分数为0、0.5%、1.0%、2.0%、4.0%时,其正磷酸铵的质量分数从未反应时的13.3%分别变为53.3%、51.5%、51.6%、52.4%、46.9%。结合一级反应动力学模型,计算发现Mg²⁺对水溶性APP的水解具有减缓作用。不同聚合度分布的水溶性APP在相同Mg²⁺浓度下正磷酸铵含量的变化量有差异,针对作物需求,应该使用不同品质的水溶性APP。     

循环冷却水系统排污水总磷超标原因分析及对策

某火力发电厂循环冷却水处理更换为低磷阻垢剂后,排污水总磷仍不能达到排放要求。通过对循环冷却水中总磷、有机磷、正磷变化规律,以及可能引起正磷含量升高的原因分析,认为排污水总磷超标是循环冷却水系统沉积物中正磷含量较高,缓慢溶出引起。采用粘泥剥离、变工况(机组负荷变化-水温变化、水质pH值变化、水体扰动)将原沉积的正磷逐步溶出,最终使循环冷却水排污水中总磷质量浓度达到0.5 mg/L的排放标准。     

Chemical Ecology Evidence for Phosphate as the Only Factor Limiting Algal Growth in Lake Kinneret

Experiments on the growth of the natural populations of algae and of other microorganisms as a function of the supply of various nutrients was carried out for Lake Kinneret water sampled at about 2 week intervals during January-June 1972. The addition of orthophosphate caused a rapid rise in biomass, which, after several days, increased to 2-5 times that in untreated water, as measured by the increase in turbidity and protein content. On the other hand, the addition of sodium or potassium nitrate, ammonium chloride, ferrous ethylenediamine sulfate, sodium silicate or vitamin B12 had no noticeable effect. The plot of biomass produced versus the concentration of added phosphate is a steeply rising function in the range of 0.1 to 1.0 μ molar orthophosphate, which levels off at higher phosphate concentrations, reaching saturation above about 2 μ molar phosphate. Thus, in the range of its natural concentration in Lake Kinneret, 0.09-0.5 μ molar, orthophosphate is the limiting factor. Above 2 μ molar phosphate, nitrate becomes the limiting factor, as was shown by experiments in which both phosphate (>2 μ molar) and nitrate were added, resulting in extremely abundant algal growth. A model of the reduction of nutrient input was achieved by laboratory experiments, in which the lake water was diluted with distilled water (by 1/4), thus resulting in an approximately proportional (to about 1/4) decrease in biomass. The effect of restoring the natural concentration of either nitrate or orthophosphate was then measured. Added nitrate had no effect, while added phosphate caused a rapid increase in biomass, which after 2-4 weeks came close to that in the natural lake water. These results indicate that during the spring of 1972, phosphorus has been the only element limiting algal growth in the lake.     

正磷酸盐的阻垢协同作用研究

采用静态阻垢法、SEM、XRD分析技术研究了PO4^3-与三元共聚物AA/AMPS/HPA对CaCO3垢的作用.结果表明：单独的PO4^3-对CaCO3无任何阻垢作用;8～20mg/LAA/AMPS/HPA＋1～6mg/LPO4^3-在阻CaCO3垢时表现出显著的协同效应,当PO4^3-质量浓度超过6 mg/L时,两者阻CaCO3的阻垢率下降,协同效应也不明显.PO4^3-与AA/AMPS/HPA三元共聚物使CaCO3的形貌发生变化,对方解石的形成有明显的抑制作用.     

金属/磷酸银复合光催化剂的研究进展

磷酸银被发现是一种具有极高活性的可见光催化剂而受到密切关注。但单独的磷酸银半导体具有稳定性差等缺点,限制了其进一步应用。梳理发现构建金属/磷酸银复合光催化剂可以实现磷酸银光生载流子的有效分离,同时还可发挥纳米金属粒子的等离子体共振效应,从而提高复合光催化剂的催化活性和稳定性,此外还可借助其他助剂构建三元复合金属/磷酸银光催化剂。本综述对磷酸银光催化剂的改性研究具有指导意义。     

Effect of Water Content on the Structure and Mechanical Properties of Magnesia-Phosphate Cement Mortar

Magnesia-phosphate cement mortars, based on magnesia and ammonium dihydrogen orthophosphate, were prepared with water contents (measured as a weight fraction of the dry material) in the range 5% to 12%. It was shown by XRD that the major reaction product was magnesium ammonium phosphate hexahydrate (MgNH₄PO₄6H₂O), also known as the mineral struvite. Evidence was also found to suggest the presence of an amorphous or poorly crystalline phase with a lower degree of hydration in materials prepared with water contents less than 8%. For higher water contents, the excess water gradually evaporated during aging to leave an interconnected fine porous structure which exhibited poor mechanical properties. An increase in the water content from 5% to 12% also led to a significant increase in the crystallite size, from around 0.5 µm to 10 µm.     

污水污泥水热炭化过程中磷的迁移转化特性

利用SMT方法研究了污水污泥水热炭化固体产物中磷的赋存形态和分布。结果表明,水热炭化处理可以使污泥中的有机磷（OP）转化为无机磷（IP）。在实验条件范围内,污泥中的磷主要富集在水热焦中（R_TP＞70%）,且主要以无机磷（IP）形态存在。延长水热炭化时间或升高水热炭化温度,污泥中无机磷（IP）和非磷灰石无机磷（NAIP）均呈逐渐升高的趋势,而且水热炭化温度的影响程度显著大于水热炭化时间。水热炭化时间对磷灰石无机磷（AP）的影响不明显,但AP含量随水热炭化温度的升高而略微升高。结合XRD谱图分析发现,105℃烘干污泥中主要存在磷酸铝盐和磷酸铁盐两种含磷化合物;水热炭化处理促使焦磷酸盐转化为正磷酸盐,且磷在水热焦中基本以最稳定的正磷酸盐形式存在。该研究结果可为污泥的资源化利用及从污泥中回收磷资源提供理论参考。     

焦磷酸盐镀铜液中正磷酸盐含量对镀层性能的影响

介绍了一种焦磷酸盐镀铜溶液中铜、总焦磷酸根、磷酸根、柠檬酸铵含量的分析方法和计算方法。分析了正磷酸根产生的原因及其危害,并给出了一种化学处理方法。对正磷酸根含量不同的镀液进行了分析,并测试了相应镀层的性能?采取了不同的措施对镀液进行改进,并对效果进行了讨论。结果表明,正磷酸根的存在是不可避免的,控制槽液温度和pH值、定期过滤溶液、补充新料等措施都可抑制正磷酸根含量的增长。     

Aluminum Phosphates Derived from Alumina and Alumina-Sol–Gel Systems

Aluminum phosphate products formed by the reactions of alumina and alumina-gel systems with acidic phosphates were analyzed. Drying of alumina-gel to form microcrystalline boehmite and conversion to γ-alumina by thermal treatment was indicated by the appearance of octahedral, pentacoordinate, or tetrahedral sites, which were established using ²⁷Al magic-angle-spinning solid-state nuclear magnetic resonance spectroscopy. Crystalline aluminum phosphate products and amorphous material were identified using this technique. α-alumina and heat-treated alumina-gel that were reacted with phosphate in an Al:P ratio of 1:1 yielded dramatically different aluminum orthophosphate:aluminum metaphosphate product ratios of 8.2:1 and 1:1.1, respectively. When alumina-gel was heat-treated with phosphate, an abundance of aluminum orthophosphate, aluminum metaphosphate, and hydrated aluminum phosphate products were affected by varying conditions of temperature and time of heat treatment and by the amount of phosphate present. An α-alumina/alumina-gel composite sol–gel phase that was reacted with phosphoric acid (H₃PO₄) in a Al:P ratio of 1:1 exhibited an increased quantity of aluminum metaphosphate products compared with an α-alumina:H₃PO₄ ratio of 1:1 and a higher percentage of reaction (79%) compared with the reactions of an α-alumina:H₃PO₄ ratio of 1:1 or an alumina-gel:H₃PO₄ ratio of 1:1. The morphologies of aluminum triphosphate hydrate and aluminum metaphosphate product phases were observed using scanning electron microscopy.