基于最小二乘支持向量机的秦皮提取工艺的研究

目的：应用最小二乘支持向量机（LS-SVM）技术优化秦皮的提取工艺。方法：以秦皮甲素和秦皮乙素为指标,采用均匀设计安排提取试验,并用最小二乘支持向量机建立关系模型。结果：最小二乘支持向量机对秦皮甲素和秦皮乙素的拟和相关系数分别为0．9997与0．9999;得到的最优工艺条件为提取温度100℃、乙醇浓度50％、液固比11、提取时间70min,机器模型在此条件下的预测值为秦皮甲素提取量为9．291mg·g^-1,秦皮乙素提取量为2．241mg·g^-1,和实际测量值的相对误差仅为-2．97％和2．66％,具有较好的预测性。结论：最小二乘支持向量机可用优化秦皮提取工艺。     

A novel preconcentration procedure using cloud point extraction for determination of lead,cobalt and copper in water and food samples using flame atomic absorption spectrometry

In this work, a new cloud point extraction (CPE) procedure was developed for the separation and preconcentration of lead(II), cobalt(II), and copper(II) in various water and food samples. Complexes of metal ions with 1-Phenylthiosemicarbazide (1-PTSC) were extracted into the surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114) from samples. After phase separation, the enriched analytes were determined by flame atomic absorption spectrometry (FAAS). Factors affecting cloud point extraction, such as pH, reagent and surfactant concentrations, temperature, and incubation time were evaluated and optimized. The interference effect of some cations and anions was also studied. After optimization of the CPE conditions, the preconcentration factor of 25 and the limits of detection (L.O.D.) obtained for lead(II), cobalt(II), and copper(II) based on three sigma (n = 20) were 3.42, 1.00, and 0.67 μg L⁻¹, respectively. The method presented precision (R.S.D.) between 1.7% and 4.8% (n = 7). The presented preconcentration procedure was applied to the determination of metal ions in reference standard materials (SRM 1515 Apple leaves and GBW 07605 Tea) and some real samples including tap water, spring water, sea water, canned fish, black tea, green tea, tomato sauce and honey.     

浊点萃取联合高效液相色谱法测定血浆中的橙皮素

目的：建立浊点萃取联合高效液相色谱法测定血浆中橙皮素的方法。方法：利用非离子型表面活性剂Triton X-114胶束水溶液萃取富集橙皮素,以甲醇-0.1%磷酸水溶液（80：20）为流动相进行洗脱,Kromasil C₁₈为色谱柱,柱温25℃,检测波长283 nm。结果：Triton X-114浓度5%、对照品溶液加入量10 μL,调pH 5,萃取温度50℃,萃取3次,每次30 min,超声5 min,所得萃取率最高,为86.6%;橙皮素在0.34~10.80 μg·mL^-1内进样量与峰面积线性关系良好,Y=94.715X+4.328 5（r=0.999 4）。结论：浊点萃取和液相色谱联用来测定血浆橙皮素,不使用有机试剂,绿色环保,简便。     

HPLC测定息痛宁胶囊中秦皮甲素和秦皮乙素的含量

目的;测定中药复方制剂息痛宁胶囊中有效成份秦皮甲素和秦皮乙素的含量。方法：采用HPLC,ODS柱,流动相为甲醇－水（24：76）,检测波长336nm。结果：秦皮甲素进样量在0．005－1．5μg范围内,峰面积与进样量有良好的线性关系,回收率99．9％;秦皮乙素进样量在0．0025－0．75μg范围内,峰面积与进样量有良好的线性关系,回收率102．7％。结论：该方法准确性高,操作简单,可供该制剂的含量测定。     

HPLC法测定九香止泻片中秦皮甲素和秦皮乙素的含量

目的:建立九香止泻片中秦皮甲素和秦皮乙素的含量测定方法。方法:采用高效液相色谱法,色谱柱为Thermo C18(250mm×4.6mm,5μm),流动相为乙腈-0.1%磷酸溶液(12∶88),流速为1.0mL·min-1,检测波长为334nm,柱温为30℃。结果:秦皮甲素进样量在80～800ng范围内与峰面积积分值呈良好线性关系(r=0.9998),平均回收率为100.1%,RSD=1.89%(n=9);秦皮乙素进样量在32.96～329.6ng范围内与峰面积积分值呈良好线性关系(r=0.9995),平均回收率为101.5%,RSD=2.42%(n=9)。结论:本法简单易行,结果准确可靠,可作为九香止泻片的含量测定方法。     

Applying cloud point extraction technique for the extraction of oxazepam from human urine as a colour or fluorescent derivative prior to spectroscopic analysis methods

Two new methods based on cloud point extraction (CPE) technique were developed and optimized for the extraction and preconcentration of oxazepam from human urine, as an azo or fluorescent derivative. The first method is a spectrophotometric one, which is based on the acid hydrolysis of the oxazepam to a benzophenone, diazotization of the benzophenone, and then the coupling with oxine to form an azo dye. The second method is a spectrofluorimetric one, which involves reduction of the target compound using Zn°/HCl at room temperature with the formation of a highly fluorescent derivative. The main factors affecting the chemical reactions and CPE were investigated and optimized systematically. Under optimum experimental conditions, the calibration graphs were linear in the range of 0.1 to 1.5 (0.05 to 2.0) μg/ml with correlation coefficients of 0.9989 (0.9985), for the CPE-spectrophotometric (CPE-spectrofluorimetric) method. The limit of detection was found to be 0.034 (0.018) μg/ml and the relative standard deviation was calculated to be 1.35 (2.52)%. Recoveries in the spiked samples ranged from 87 to 94%. Finally, the proposed methods were applied to the determination of oxazepam in human urine.     

浊点萃取法提取青蒿中青蒿素的工艺研究

目的优选浊点萃取法提取青蒿中青蒿素的最佳工艺。方法采用浊点萃取法提取青蒿素,并用紫外分光光度法测定含量。用正交试验法确定表面活性剂浓度、离子强度、液固比、平衡时间等因素对提取率的影响,优选最佳提取工艺。结果采用非离子表面活性剂聚氧乙烯脂肪醇醚(Genapol-X 80),浓度为15.0%,液固比为100∶1,NaCl浓度为2.0 mol/L,在60℃下萃取40 min,可达到最高的提取率。相对于传统工艺,浊点萃取法的提取率大大提高。结论该方法稳定易行,且操作简单、绿色环保、避免高温破坏、提取率高。     

正交试验优选白头翁汤提取工艺

目的:优选白头翁汤提取工艺。方法:以乙醇浓度、乙醇用量、提取次数和提取时间为考察因素,以浸膏得率和白头翁皂苷B_4、秦皮甲素、秦皮乙素、小檗碱的含量为指标,采用L_9(3~1)正交设计优选最佳提取工艺。结果:最佳提取工艺为8倍量60%乙醇,提取3次,每次1.5 h结论:优选的提取工艺稳定、可行。     

浊点萃取法提取贯叶连翘总黄酮的研究

目的建立浊点萃取提取贯叶连翘中总黄酮的工艺。方法采用浊点萃取法进行总黄酮提取,并用紫外分光光度法测定其含量。用正交实验法确定表面活性剂质量浓度、液固比、离子强度、平衡时间等关键因素对提取率的影响,优化提取工艺。结果采用非离子表面活性剂聚氧乙烯脂肪醇醚Genapol-X 80,质量浓度为50.0g.L-1,液固比为100∶1,NaCl浓度为3.0mol.L-1,在65℃下,萃取40min,达到最高的提取率,相对于传统工艺,提取率大大提高。结论该方法稳定易行,操作简单,绿色环保,避免高温破坏,提取率高。     

Indirect fibre‐optic colorimetric determination of ascorbic acid using 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol and cloud point extraction

A new method has been developed for the indirect determination of ascorbic acid (AA) in commercial syrup preparations based on cloud point extraction (CPE) separation and preconcentration, and determination by molecular absorption spectrometry. The colorimetric method was based on the reduction of Fe(III) to Fe(II) and complexation of Fe(II) with 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol (Br‐PADAP), followed by its extraction into Triton X‐114. Selectivity of the method was increased with the use of EDTA as a masking agent. The absorbance was measured at 742 nm. Various influencing factors on the separation and preconcentration of AA have been investigated systematically, and the optimized operation conditions were established. The proposed method allows the determination of AA in the range 5–200 µg L^?1 with a relative standard deviation of 3.0%. The detection limit was found to be 0.9 µg L^?1 for AA. This method has been applied to the determination of ascorbic acid in commercial pharmaceutical preparations. Copyright © 2011 John Wiley & Sons, Ltd.     

膝可保胶囊质量标准分析与研究

目的：建立膝可保胶囊的质量标准。方法：采用薄层色谱法对膝可保胶囊中秦皮、龙血竭药材进行鉴别;采用高效液相色谱法对膝可保胶囊中芍药苷、秦皮甲素、秦皮乙素进行含量测定。结果：薄层色谱专属性强,分离度高,阴性对照无干扰;高效液相色谱法测得秦皮甲素、秦皮乙素、芍药苷分别在0.123 6～0.865 2 μg（r=0.999 6）,0.075 9～0.531 3 μg（r=0.999 6）,0.060 6～1.515 0 μg（r=0.9995）范围内进样量与峰面积呈良好的线性关系,平均加样回收率分别为98.85%,98.41%,99.59%,RSD分别为1.89%,1.91%,1.28%。结论：所建立的定性、定量方法操作简便,结果准确,重现性好,能够有效控制膝可保胶囊的质量。     

Simultaneous determination of dysprosium and iron in urine by capillary zone electrophoresis coupled to cloud point extraction

Automated preconcentration strategies are needed when analyzing metals in real samples by capillary electrophoresis (CE) with UV detection. The on-line incorporation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with CE for simultaneously determining dysprosium and iron at ppb levels in urine is presented and evaluated for the first time. The preconcentration step is mediated by micelles of the non-ionic surfactant polyethyleneglycol-mono-p-nonylphenylether (PONPE 7.5) with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol. The micellar system containing the complex was loaded into the FIA manifold at a flow rate of 8 mlmin(-1), and the surfactant rich-phase was retained in a microcolumn packed with cotton, at pH 9.2. The surfactant-rich phase was eluted with 50 microl acetonitrile directly into the CE sample vial, allowing to reach an enrichment factor of 200-fold for a 10 ml sample urine. The type and composition of the background electrolytes (BGE) were investigated with respect to separation selectivity, reproducibility and stability. A BGE of 20mM sodium tetraborate buffer containing 13% acetonitrile, pH 9.0 was found to be optimal for the separation of metal chelates. Detection was performed at 585 nm. An enhancement factor of 200 was obtained for the preconcentration of 10 ml of sample solution. The detection limits for the preconcentration of 10 ml of urine were 0.20 microgl(-1) for Dy, and. 0.48 microgl(-1) for Fe. The calibration graphs using the preconcentration system were linear with a correlation coefficient of 0.9989 (Dy) and 0.9976 (Fe) at levels near the detection limits up to at least 500 microgl(-1). The method was successfully applied to the determination of dysprosium and iron in urine for monitoring the elimination of dysprosium-based pharmaceuticals.     

Total mercury determination in different tissues of broiler chicken by using cloud point extraction and cold vapor atomic absorption spectrometry

A cloud point extraction (CPE) method has been developed for the determination of total mercury (Hg) in different tissues of broiler chicken by cold vapor atomic absorption spectrometry (CVAAS). The broiler chicken tissues (leg, breast, liver and heart) were subjected to microwave assisted digestion in a mixture of nitric acid and hydrogen peroxide (2:1 ratio), prior to preconcentration by CPE. Various parameters such as the amount of ammonium O,O-diethyldithiophosphate (DDTP), concentrations of Triton X-114, equilibrium temperature, time and centrifugation have been studied in order to find the best conditions for the determination of mercury. For validation of proposed method a certified reference material, DORM-2 was used. No significant difference p > 0.05 was observed between the experimental results and the certified values of CRM (paired t-test). The limit of detection and quantitation obtained under the optimal conditions were 0.117 and 0.382 μg/kg, respectively. The accumulation of Hg in different tissues were found in the order of, liver > muscles > heart. The concentration of Hg in chicken tissues were found in the range of 1.57–2.75, 1.40–2.27, 1.55–4.22, and 1.39–2.61 μg/kg in leg, breast, liver and heart, respectively.     

正交试验优选痛风胶囊提取工艺

目的:优选痛风胶囊的最佳提取工艺条件。方法:以大黄素、大黄酚、秦皮甲素、秦皮乙素含量结合出膏量为考察指标,采用正交设计法,对溶剂浓度、溶剂用量、提取时间和提取次数等影响因素进行优选。结果:最佳提取工艺条件为:药材分别加70%乙醇7倍量,提取2次,每次2 h。结论:该工艺稳定、可行,提取率高。     

微乳液相色谱法测定大鼠血浆中罗布麻甲素的浓度及其药动学研究

目的：建立测定大鼠血浆中罗布麻甲素的微乳液相色谱方法,并将其用于大鼠体内药动学的研究。方法：用微乳液相色谱法分别测定给药后不同时间点大鼠的血药浓度,并对其药动学参数进行研究。色谱条件为：色谱柱为Zorbax SB-C₁₈（150 mm×4.6 mm,5 μm）柱;流速0.8 mL·min^-1;检测波长360 nm;柱温30℃。采用经过优化后的微乳体系为流动相,其组成为：2.0% Genapol X-080-2.8%正丁醇-1.8%乙酸乙酯-0.4%三乙胺-93.0%水溶液（pH调至5.0）。结果：大鼠静脉注射罗布麻甲素后,其药动学模型符合二室模型。分布和消除相半衰期分别为7.3 min和28.7 min。药时曲线下面积AUC（μg·min^-1·mL^-1）为804.37。表观分布容积V_d（μg·mL^-1）为0.325。平均驻留时间MRT（min）为25.8。大鼠血浆中罗布麻甲素在0.1~10 μg·mL^-1内线性均良好（r=0.998 6）,最低定量浓度（S/N=10）为0.1 μg·mL^-1,日内和日间RSD均小于4.9%,平均加样回收率在96.3%~98.8%之间,RSD均小于5.1%。结论：本法快速、简便、准确、重现性好,可用于罗布麻甲素血药浓度测定及药动学研究。     

浊点萃取－气相色谱法测定水中邻苯二甲酸酯类化合物

目的：建立浊点萃取－异辛烷反萃取－气相色谱测定水中3种邻苯二甲酸酯类化合物的方法。方法取水样品0．5mL，加入适量萃取剂Triton X－114、添加剂NaCl，置于45℃水浴中加热，离心后，放入冰水浴中冷却，弃水相，加入异辛烷，超声，离心，取上层异辛烷相进气相色谱检测。结果在优化的实验条件下，3种化合物能够达到较好分离，在0．0002～0．005 mg? mL －1浓度范围内均呈现良好的线性，方法的加标回收率均达97％以上，相对标准偏差均小于5％。结论本方法可用于分离检测水中邻苯二甲酸酯类化合物，具有准确、简捷等特点。     

Effect of manufacturing parameters on the characteristics of vitamin C encapsulated tripolyphosphate-chitosan microspheres prepared by spray-drying

To prepare the sustained release vitamin C carriers, vitamin C was successfully encapsulated in tripolyphosphate (TPP) cross-linked chitosan (TPP-chitosan) microspheres by the spray-drying method at different manufacturing conditions. Manufacturing parameters (inlet temperature, liquid flow rate, chitosan concentration and volume of 1% w/v TPP solution) had a significant influence on the characteristics of thus prepared microspheres. The optimum spray-drying conditions such as inlet temperature, liquid flow rate and compressed air flow rate for the encapsulation of vitamin C in TPP-chitosan microspheres was found to be 170 degrees C, 2 ml min(-1) and 101 min(-1), respectively. The size and yield of the TPP-chitosan microspheres ranged from 3.9-7.3 microm and 54.5-67.5%, respectively. The encapsulation efficiency of TPP-chitosan microspheres ranged from 45.72-68.7% and it decreased with the increasing volume of 1% w/v TPP solution. At the same cross-linking extent, the encapsulation efficiency of TPP-chitosan microspheres increased when the concentration of chitosan was increased from 0.5-1% w/v. Effect of volume of 1% w/v TPP solution on the surface morphology of chitosan microspheres was examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). These studies revealed that chitosan solution (250 ml) cross-linked with 15 ml 1% w/v TPP solution produced more porous microspheres than that cross-linked with 5 and 10 ml TPP solution. The release rate of vitamin C from TPP-chitosan microspheres decreased when the concentration of chitosan was increased from 0.5-1.0% w/v. Vitamin C release rate was also modulated by varying the volume of 1% w/v TPP solution. The release rate of vitamin C from TPP-chitosan microspheres decreased with increasing volume (5-15 ml) of 1% w/v TPP solution.     

HPLC测定菊苣药材中的有效成分

目的 测定菊苣药材中有效成分的含量.方法 采用HPLC法.结果 秦皮甲素、秦皮乙素、山莴苣苦素、羽扇豆醇的回收率分别为102.01%、102.99%、102.86%、101.06%,RSD分别为2.84%、2.60%、1.12%、2.47%,其回归方程的相关系数分别为0.9995、0.9998、0.9996、0.9992.结论 所用方法准确、快速、简便、重复性好,可用于菊苣有效成分的含量测定.     

HPLC法同时测定加味白头翁汤凝胶灌肠剂中秦皮甲素和盐酸小檗碱的含量

目的：建立反相高效液相色谱法同时测定医院制剂加味白头翁汤凝胶灌肠剂中秦皮甲素和盐酸小檗碱的含量。方法：色谱柱为DiamonsilC18（250mm×4.6mm,5μm）;采用梯度洗脱的方法,流动相：溶液A为乙腈,溶液B为含5%三乙胺的0.33mol·L^-1磷酸二氢钾缓冲液（pH=3.0）。0～9min,溶液A：溶液B为12∶88;9～10min,A∶B为30∶70;10～22min,A∶B为30∶70。流速：1.0mL·min^-1;秦皮甲素和盐酸小檗碱的检测波长分别为334nm和349nm。结果：秦皮甲素和盐酸小檗碱分别在4～200μg·mL^-1和1～50μg·mL^-1范围内线性良好;平均加样回收率分别为96.63%（RSD=2.52%）和97.37%（RSD=1.84%）。结论：本方法准确、重现性好,可用于加味白头翁汤凝胶灌肠剂的质量控制。     

Determination of quetiapine and its metabolites in plasma by field-enhanced sample stacking

Quetiapine is an atypical antipsychotic drug that can be used to treat mental disorders, including schizophrenia, bipolar disorder and Alzheimer’s disease. Quetiapine is mainly converted into the active metabolites of norquetiapine and 7-hydroxyquetiapine by the liver enzymes CYP3A4 and CYP2D6. In this study, liquid-liquid extraction (LLE) was used as a sample pretreatment method to eliminate interferences in plasma. tert-Butyl methyl ether was chosen as the extraction solvent. Field-enhanced sample injection (FESS), an online preconcentration technique, was used to analyze quetiapine and its metabolites norquetiapine and 7-hydroxyquetiapine in plasma. The optimal separation condition was 120 mM phosphate (pH 4.0) containing 0.005% (w/v) polyvinyl pyrrolidone and 40% (v/v) methanol. The methanol plug was 0.3 psi for 6 s, the sample was electrokinetic injection by 10 kV for 60 s at positive polarity, and the separation voltage was set at 26 kV. In this experiment, quetiapine, norquetiapine and 7-hydroxyquetiapine were successfully extracted from plasma by the LLE method and stacking and separated by FESS within 15 min. The limits of detection (S/N = 3) of quetiapine, norquetiapine and 7-hydroxyquetiapine were 0.25 ng/mL, 0.50 ng/mL and 1.00 ng/mL, respectively. The linear ranges of quetiapine, norquetiapine and 7-hydroxyquetiapine were 3–120 ng/mL and the correlation coefficients were 0.999. Compared with that of the traditional capillary zone electrophoresis method, the sensitivity enrichment of analytes was 463-835-fold. The optimal experimental conditions were successfully applied to the analysis of plasma samples from patients taking quetiapine for the treatment of schizophrenia.