HPLC法测定消斑颗粒中补骨脂素、异补骨脂素含量

目的采用HPLC法测定消斑颗粒中补骨脂素、异补骨脂素含量.方法色谱柱为Dikma ODS-C18色谱柱,乙腈-0.025 mol/L磷酸水溶液(30:70)为流动相,检测波长为246 nm.结果供试溶液中补骨脂素、异补骨脂素与相邻组分分离度良好,阴性液无干扰.方法重复性、稳定性、精密度、回收率试验均符合有关规定.结论方法简单、快捷、精确,可作为消斑颗粒质量控制方法之一.     

超临界流体色谱分离纯化补骨脂中的异补骨脂素和补骨脂素

建立超临界流体色谱(SFC)分离纯化补骨脂中异补骨脂素和补骨脂素的工艺方法。采用YMC-C_(18)、YMC-Diol和YMC-NH_2等3种色谱柱,甲醇、乙腈、乙醇、异丙醇等4种改性剂,流动相流速2～6 mL×min~(-1)、温度300～325 K、压力10～14 MPa条件下,考察了异补骨脂素和补骨脂素的纯化效果。放大得到制备型SFC条件为:色谱柱YMC-Diol;流动相为含有j=2%甲醇的超临界二氧化碳,流速14.0 mL×min~(-1);分离温度313 K;压力12 MPa。结果表明,分离得到的异补骨脂素和补骨脂素的纯度均大于98%,由Van’t Hoff曲线可知实验条件下SFC分离过程为焓控过程。     

不同选择性的C18检测全鹿丸中补骨脂素和异补骨脂素含量

研究了用不同键合工艺的C18柱在药典要求的流动相条件下对全鹿丸中目标物进行分离的不同效果,通过使用不同选择性的色谱柱对全鹿丸中的补骨脂素和异补骨脂素进行含量测定,建立了高效液相色谱法测定中药成分全鹿丸中补骨脂素和异补骨脂素的方法。方法简便、灵敏、准确、重现性好、分析时间短,满足药企对全鹿丸的质量控制要求。     

HPLC法测定壮肾丸中补骨脂素、异补骨脂素的含量

建立了用HPLC法测定壮肾丸中补骨脂素、异补骨脂素含量的方法.采用Agilent 1100 series高效液相色谱仪C<,18>柱,以乙腈-0.125%磷酸(25:75)为流动相,检测波长247nm.补骨脂素的线性范围为0.026～0.26 μg,r=0.999 9,平均回收率为98.8%:异补骨脂素的线性范围为0.024 56～0.2 456 μg,r=0.999 9,平均回收率为101.9%.本方法简便、准确,可用于控制该制剂的质量.     

RP-HPLC-PDA同时测定中药中补骨脂素和异补骨脂素含量

建立了中药中补骨脂素、异补骨脂素的高效液相色谱分析方法。采用的色谱条件为:Symmetry C18色谱柱(4.6mm×250mm,5μm),用乙腈-水(30:70)作为流动相,检测波长为246 nm,流动相流速为1.0m L/min,柱温为35℃。补骨脂素和异补骨脂素的浓度在3~30μg/m L时,组分的峰面积与浓度之间的线性关系良好,补骨脂素的线性方程为A=26983C+12603(C单位:μg/m L),R~2=0.9998,异补骨脂素的线性方程为A=29208C+10084(C单位:μg/m L),R~2=0.9997,回收率在97.6%~103.3%,精密度良好,补骨脂素、异补骨脂素的RSD值分别为0.718%、0.810%。方法简便,快速,适用于补骨脂素和异补骨脂素的同时测定,中药补骨脂和中成药驱白巴布期片中补骨脂素和异补骨脂素含量存在差异。     

柑橘精油中呋喃香豆素的超高效液相色谱分析

建立了柑橘类精油中4种呋喃香豆素(异补骨脂素、补骨脂素、5-甲氧基补骨脂素和欧前胡素)的超高效液相色谱(UPLC)分析方法。样品经甲醇稀释定容,高速离心分离后,取上清液进样分析。采用Agilent Zorbax Eclipse Plus C18色谱柱(2.1 mm×50 mm,1.8μm)分离,以水-乙腈二元流动相梯度洗脱,流速0.3 m L·min-1,检测波长300 nm。4种呋喃香豆素在0.5~100 mg·L-1范围内呈良好线性,相关系数均达到0.999,检出限为1.5~3.0 mg·kg-1,平均回收率为97.5%~105.6%,相对标准偏差为0.4%~2.9%(n=3)。采用已建立的方法对25批柑橘类精油样品进行测定,发现1个批次的甜圆柚油中含有5-甲氧基补骨脂素,质量分数为60.5 mg·kg-1。     

异补骨脂素酰胺类化合物的合成及其AKR1C3抑制活性

以7-羟基香豆素为初始原料，经Duff甲酰化反应、Rap-Stoermer反应、水解反应和缩合反应得具有酰胺侧链的角型呋喃香豆素(异补骨脂素)类化合物；利用HR-MS、¹HNMR及¹³CNMR确证化合物的结构；通过中通量抑酶活性测试方法评价化合物对AKR1C3及AKR1C1的抑制作用。合成了7个新的异补骨脂素酰胺类化合物；初步酶活性测试结果显示，N,N-二正丙基-4-甲基-2-氧-2H-呋喃并[2,3-h]色烯-8-甲酰胺对AKR1C3具有一定的选择性抑制作用。采用上述方法可成功合成异补骨脂素酰胺类化合物，化合物5e具有一定的选择性AKR1C3抑制作用，可为后续研究提供一定的依据。     

无花果叶中补骨脂素的分离纯化工艺研究

研究了大孔树脂分离纯化无花果叶中补骨脂素的工艺条件及树脂前处理的方法。以补骨脂素洗脱率和纯度为考察指标,确定DM101型大孔吸附树脂分离纯化补骨脂素的吸附性能和洗脱参数,建立用紫外分光光度法进行大孔树脂前处理的方法。结果表明,DM101型大孔吸附树脂吸附容量以干树脂计为9.76mg·g~(-1),用纯化水和不同浓度的乙醇依次洗脱,以60%乙醇洗脱效果最佳,洗脱率达90.76%,总干燥物中补骨脂素含量达69.28%。大孔吸附树脂对补骨脂素有较好的分离纯化作用,且工艺简单,成本低,易于工业化生产。     

高效液相色谱法测定化妆品中香豆素类化合物

建立了化妆品中8-羟基补骨脂素、补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、三甲沙林、欧前胡素、异欧前胡素8种香豆素类化合物含量鉴定的高效液相色谱分析方法。样品经超临界CO2萃取法提取,其中以甲醇作为载体助溶剂。采用Agilent?ZORBAX?Eclipse?Plus?C18色谱柱?(250?mm×4.6?mm×5?μm)作为分析柱,乙腈和水作为二元流动相,柱温25?℃,流速1.0?mL/min,检测波长250?nm,外标法定量。结果表明,8种化合物的线性相关系数均大于0.999,低、中、高3种加标水平下的平均加标回收率为85.1%～110.0%,相对标准偏差RSD6.42%?(n=6)。该方法简单、高效、准确,为化妆品中香豆素类化合物定量提供了一种有效的分析技术。     

HPLC法同时测定化妆品中补骨脂素、异补骨脂素、新补骨脂异黄酮和补骨脂二氢黄酮含量

采用高效液相色谱法研究了化妆品中补骨脂素、异补骨脂素、新补骨脂异黄酮和补骨脂二氢黄酮的含量测定,得到了补骨脂素、异补骨脂素、新补骨脂异黄酮和补骨脂二氢黄酮分别在0.109 1～21.814 4 mg/L、0.106 7～21.332 8 mg/L、0.108 6～21.712 8 mg/L、0.112 3～22.464 4 mg/L范围内线性关系良好,平均回收率为94.78%～104.74%,RSD均小于5%。     

Comparative metabolism of [3H]psoralen and [3H]isopsoralen by black swallowtail (Papilio polyxenes Fabr.) caterpillars

The comparative fate of tritiated preparations of a linear furanocoumarin (psoralen) and an angular furanocoumarin (isopsoralen) was determined in last-instar caterpillars of the black swallowtail butterfly (Papilio polyxenes Fabr.). Oral administration of either furanocoumarin at 5 g/g is followed by rapid metabolism, primarily through oxidative cleavage of the furan ring, and the metabolites are rapidly excreted. Isopsoralen is, however, metabolized at a somewhat slower rate than is psoralen, and levels of unmetabolized isopsoralen in body tissues of the treated caterpillars are about three-fold higher. These data are compatible with the hypothesis that a reduced detoxification rate accounts at least in part for the susceptibility ofP. polyxenes caterpillars to the deleterious effect of isopsoralens.     

Psoralen and Isopsoralen’s Cloud-Point Extraction from Psoralea corylifolia L.

A novel separation method based on micelle-mediated extraction and cloud-point preconcentration was developed for the hydrophobic compounds of psoralen and isopsoralen from Psoralea corylifolia L. by high performance liquid chromatography with photodiode array detection. The GENAPOL X080 was chosen as the extract surfactant. A series of experimental conditions were probed to optimize the extraction and preconcentration process. The optimized technique is a cheap, simple, and sensitive method.     

补骨脂抗癌成分的分离与鉴定

从中药补骨脂 (Psoraleacorylifolia)种子中通过溶剂提取、硅胶柱层析、SephadexLH 2 0柱层析和制备薄层层析等方法分得 4个化合物。波谱分析 (核磁共振氢谱、碳谱和质谱 )确定它们的结构分别为补骨脂素 ( 1,psoralen)、异补骨脂素 ( 2 ,isopsoralen)、补骨脂定 ( 3 ,psoralidin)和异补骨脂查尔酮 ( 4 ,isobavachalcone)。文献报道化合物 1～ 3有不同程度的抗癌作用     

Fate of photosensitizing furanocoumarins in tolerant and sensitive insects

The fate of [¹⁴C]xanthotoxin (8-methoxypsoralen) was studied in larvae of insect species that are tolerant (Papilio polyxenes Stoll) or sensitive (Spodoptera frugiperda J.E. Smith) to the phototoxic effects of photosensitizing psoralens. Both insects metabolize xanthotoxin by oxidative cleavage of the furan ring, but the detoxification occurs at a much more rapid rate inP. polyxenes in which >95% of an oral 5 g/g xanthotoxin dose is metabolized within 1.5 hr after treatment. The detoxification of psoralens byP. polyxenes appears to occur primarily in the midgut tissue prior to absorption, with the result that the intact phototoxin does not reach appreciable levels in body tissues. Studies with an angular furanocoumarin indicated that isopsoralens are metabolized byP. polyxenes at a somewhat slower rate than observed for psoralens; however, a reduced rate of metabolic detoxification of isopsoralens probably does not explain the fact that psoralen tolerance inP. polyxenes does not extend to the isopsoralen series.     

热敏型薄荷油加香颗粒的制备工艺优化

采用挤出滚圆技术制备玉米多孔淀粉颗粒,将热敏性微胶囊薄荷油膏体分散于该颗粒上,平衡后制得滤嘴用热敏型薄荷油加香颗粒,运用高效液棚色谱和顶空气相色谱测定其释放挥发率和包封率,经单因素和正交试验筛选及优化制备工艺参数。试验结果表明．最佳制备工艺为A3D3C1B2,即玉米多孔淀粉与羟丙基甲基纤维索的质量比为200：1。孔板直径为0．45mm,螺杆转速为30r／min,水的质量分数为25％。由此制备的颗粒的产率为（85．3±1）％．释放挥发率为（56．68±0．1）％,综合评价得分为（68．14±1）分,热分析表明该加香颗粒在40－50℃具有较好的释放效果,能够温和释放溥倚油．适用于滤嘴加香。     

The effect of powder size on induction behaviour and binder distribution during high shear melt agglomeration of calcium carbonate

Growth mechanisms in high shear mixer granulation were observed over a wide range of particle size and liquid-to-solid (L/S) ratio. The materials used were calcium carbonate (CaCO₃; size fractions in the range 1.5 to 85 μm) with a binder of polyethylene glycol 6000 (PEG 6k). The binder, solid at room temperature, was added by the “melt-in” method. A 10 L vertical-axis granulator was used, with a chopper and a four-bladed impeller.

The mean granule size and granule size distribution were measured at regular intervals during the agglomeration process by careful sampling and sieving. The uniformity of binder distribution among the granules was also measured.

The growth behaviours of each grade of primary particles were classified and compared. An induction type mechanism was observed with an initial period of slow growth in mean particle size that lasted 2 to 3 min (the induction period). This was followed by a short rapid growth phase lasting 1 to 2 min. The final stage was a plateau of more or less zero growth. Interestingly, the end of the induction period and the onset of rapid growth corresponded to a change in the granule size distribution from bimodal to monomodal and a similar change in the distribution of binder. Induction period growth rate tended to be lower for granules of finer particles, but these grew more rapidly during the rapid growth stage and produced larger granules than the coarser primary particles.

The liquid-to-solid (L/S) ratio had a significant effect on the growth rate during the rapid growth stage but a minor effect on the granule size distribution and binder distribution. Primary particle size had a significant effect on the final average size of granules, the growth rate during the rapid growth stage and the distribution of granule size and binder.     

常温下微细化淀粉的制备

利用硫酸水解的方法。在常温情况下制备微细玉米淀粉颗粒。结果表明：在20℃条件下用浓度为4mol／L的硫酸,反应72h,水解效果最好。通过控制反应条件。研究了盐酸、硫酸浓度、反应时间对淀粉颗粒平均粒径的影响,并优化反应工艺条件。     

双波长扫描法测定蚂蚁乙肝宁散剂中黄芪甲甙含量

采用双波长扫描测定蚂蚁乙肝宁散剂中黄芪甲甙含量，经方法学考察，其重现性、稳定性均良好，回收率为９７．４％，ＲＳＤ为１．７％，为该制剂质量分析提供了可行的方法。     

PVC塑料中增塑剂测定影响因素的探讨

在检测聚氯乙烯（ PVC）中增塑剂含量常用的检测方法有CPSC-CH-C1001-09.3、 GB/T 22048-2008、 EN 14372：2004,以上方法对样品制备的粒径要求各异,本文通过对PVC塑料5 mm,2 mm和〈1 mm三种粒径进行比对测试,结果表明按标准要求制备的粒径对CPSC-CH-C1001-09.3、 GB/T 22048-2008的检测方法没有影响;对EN 14372：2004检测方法影响很大,粒径越小,检出率越高。 PVC增塑剂的萃取效果除了与粒径大小相关之外,还与萃取溶剂的极性有关系,溶剂极性越大,萃取时间越短。     

Optimization of a Fe-Al-Ce nano-adsorbent granulation process that used spray coating in a fluidized bed for fluoride removal from drinking water

A coating granulation technology comprising the spraying of a Fe-Al-Ce nano-adsorbent suspension onto glass beads in a fluidized bed was developed. An acrylic-styrene copolymer latex was used as a binder. The granulated adsorbent was used in a packed bed for fluoride removal from drinking water. The effects of coating temperature, latex/Fe-Al-Ce ratio, and coating amount on granule compressive strength and adsorption capacity were investigated. With increased coating temperature, cross linking in the polymer in the coated layer increased, which resulted in increased granule strength but decreased adsorption capacity. With increased latex/Fe-Al-Ce ratio, more active sites were covered by the polymer, which also resulted in increased granule strength but decreased adsorption capacity. The optimal parameters for making high performance adsorbent granules were for the granules to be coated at 65 °C using a latex/Fe-Al-Ce ratio of 0.5:1 and a coating amount of 27.8%. These granules had a fluoride adsorption capacity of 2.77 mg/g (coated granules) for water with an initial fluoride concentration of 0.001 M that was treated at pH 7.