HPLC同时测定丹酚酸B和阿魏酸的含量

目的 建立HPLC同时测定丹酚酸B和阿魏酸的方法。方法 色谱柱ODS-C₁₈(4.6 mm×250 mm,5 μm)柱,流动相：甲醇-乙腈-甲酸-水,检测波长为286 nm,流速0.8 mL·min^-1。结果 丹酚酸B浓度在5.40~43.25 μg·mL^-1,阿魏酸浓度在3.37~27.00 μg·mL^-1内线性关系良好。丹酚酸B和阿魏酸的线性方程分别为：Y=0.971 1X-2.215 4,r=0.999 8,Y=0.415 9X-0.450 7,r=0.999 9;平均回收率分别为98.4%,98.7%;RSD分别为3.39%,1.49%。结论 本法在检测丹酚酸B和阿魏酸时有较好的专属性,灵敏度高,重复性好,且样品处理简单、容易操作,可以作为丹参和当归复方制剂的质量检测方法。     

HPLC法测定癃闭舒片中补骨脂素和异补骨脂素

目的 建立癃闭舒片中补骨脂素和异补骨脂素的定量方法。方法 对国内3个企业生产的6个批次的癃闭舒片,采用HPLC法检测,Agilent TC-C₁₈(2)色谱柱(250 mm×4.6 mm,5μm),流动相是甲醇-水(43:57),体积流量1.0 mL/min,检测波长为246 nm,柱温30℃。结果 补骨脂素回归方程为:Y=84.44X+9.994,r=0.9999(n=12)。异补骨脂素回归方程为:Y=82.434X+8.8952,r=0.9999(n=12)。补骨脂素和异补骨脂素的线性范围均在4.04~151.5μg。结论 本方法操作简便、准确、专属性强、稳定,可用于癃闭舒片中补骨脂素和异补骨脂素的含量测定。     

用LC-MS/MS法同时测定栀子中3种环烯醚萜苷类成分的含量

目的 建立同时测定栀子中3种环烯醚萜苷类成分含量的方法。方法 采用液相色谱-串联质谱（LC-MS/MS）法。色谱条件：Dikma Diamonsil^® C₁₈柱（100 mm×4.6 mm,5 μm）;流动相为0.1%乙酸水（A）-0.1%乙酸乙腈（B）,梯度洗脱;流速为0.4 ml/min;柱温40℃;进样量2 μl。质谱条件：电喷雾离子化电离源（ESI）,正/负离子检测,雾化气流量3 L/min,干燥气流量15 L/min,脱溶剂管温度240℃,加热块温度400℃,碰撞气压力230 kPa,以多反应监测模式（MRM）配对离子方式进行定量,山栀苷、京尼平龙胆双糖苷、栀子苷选择的离子对质荷比分别为m/z 391.10→149.30,m/z 573.40→365.05,m/z 447.30→225.15。结果 回归方程为：山栀苷Y=243.810X-289.957,r=0.999 9;京尼平龙胆双糖苷Y=137.125X+2 092.76,r=0.999 6;栀子苷Y=2 030.32X+823 213,r=0.999 8;线性范围分别为10.76~2 152 ng/ml、516~4 128 ng/ml、2 000~20 000 ng/ml。精密度、稳定性、重复性和加样回收率试验结果均符合要求。结论 此方法可快速、准确、灵敏地测定栀子中3种环烯醚萜苷类成分的含量,为栀子的质量控制提供依据。     

HPLC法测定扶正平消胶囊中芍药苷的含量

目的 建立扶正平消胶囊中芍药苷含量的测定标准。方法 采用HPLC法进行含量测定,色谱柱为Agilent Zorbax SB-C₁₈柱（150 mm×4.6 mm,5 μm）,流动相：乙腈-5 mmol/L磷酸二氢钠水溶液（10：90）,流速：1.0 ml/min,柱温：25℃;检测波长：230 nm,进样量10 μl,运行时间25 min。结果 芍药苷在25.0~500.0 μg/ml范围内线性关系良好（r=0.999 9）,线性方程：Y=12.65X+43.54,平均加样回收率为92.69%,RSD为1.77%。结论 该方法操作易行、结果可靠、重复性好,可用于扶正平消胶囊中芍药苷的含量测定。     

HPLC同时测定瑞香狼毒中瑞香素、伞形花内酯和东莨菪内酯的含量

目的 建立HPLC同时测定瑞香狼毒中瑞香素、伞形花内酯和东莨菪内酯含量的方法。方法 样品经无水乙醇回流。采用Synergi 4u Polar-RP 80R柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-1%冰醋酸溶液,等度洗脱,流速：1.0 mL·min^-1,检测波长：324 nm,柱温：30℃。结果 瑞香素在0.012~0.250 μg（r=0.999 9）、伞形花内酯在0.149~2.981 μg（r=0.999 9）、东莨菪内酯在0.012~0.239 μg（r=0.999 9）均呈良好的线性关系;瑞香素、伞形花内酯和东莨菪内酯的加样回收率分别为99.0%（RSD=0.94%）,98.7%（RSD=0.77%）和98.3%（RSD=1.16%）。结论 3种香豆素成分在35 min内达到基线分离,该方法分析时间短、稳定性和回收率良好,对瑞香狼毒药材的质量控制具有一定的参考价值。     

原子吸收光谱法和原子荧光光谱法测定蜂产品中的重金属残留量

目的 建立不同种类蜂产品中铅、砷、汞的重金属残留量的检测方法。方法 采用微波消解法处理蜂产品,通过选择最佳消解条件和测定条件,利用石墨炉原子吸收光谱法测定蜂产品中铅含量,和利用原子荧光光谱法测定蜂产品中砷、汞含量,并对测定方法进行方法学考察。结果 铅、砷、汞测定方法线性关系分别为Y=0.003 04X+0.001 31（r=0.999 6）、Y=88.645 1X＋2.563 8（r=0.999 9）、Y=552.113 2X-6.169 5（r=0.999 6）,RSD均<3%,回收率分别为98.2%,96.3%,93.8%,测定结果分别为0.003~4.203,0~0.192,0~0.097 6 mg·kg^-1。结论 不同种类蜂产品中重金属含量不同,其中铅含量最高,本方法适用于同时检测蜂产品中多种重金属残留。     

啤酒花中黄酮类成分的含量分析

目的 建立啤酒花中总黄酮和黄腐酚含量测定方法,对来自不同产地和品种的29个啤酒花样品中的总黄酮和黄腐酚进行测定。方法 用芦丁-AlCl₃分光光度法测定总黄酮的含量;用HPLC-UV法测定黄腐酚的含量。色谱条件：色谱柱为Dikma Technologies Diamonsil C₁₈柱（250 mm×4.6 mm,5 μm）;流动相为乙腈-1%冰醋酸梯度洗脱,流速为1.0 ml/min;柱温为25℃;检测波长为370 nm。结果 总黄酮回归方程为A=30.345C+0.016 8,r=0.999 9;黄腐酚回归方程为A=55 446C+9 040.5,r=0.999 9,表明总黄酮在20.2~404.0 μg/ml,黄腐酚在2.152~43.040 μg/ml范围内,线性关系良好,两者精密度和重复性RSD均<2%,平均加样回收率分别为102.71%和100.21%。结论 不同种类的啤酒花之间,总黄酮和黄腐酚含量存在巨大差异,进口啤酒花优于国产。     

HPLC同时测定斑蝥酸钠维生素B6注射液中斑蝥酸钠和维生素B6的含量

目的 建立斑蝥酸钠维生素B₆注射液中斑蝥酸钠和维生素B₆含量的同时测定方法。方法 采用HPLC，色谱柱为Syncronis C₁₈（250 mm×4.6 mm，5 μm），流动相为0.02 mol·L^-1磷酸二氢钾溶液（磷酸调pH值至2.6）-乙腈，梯度洗脱，流速为1.0 mL·min^-1，检测波长为193，290 nm，波长切换法，柱温：30℃。结果 斑蝥酸钠回归方程为Y=1.926X+0.010（r=0.999 7），在0.064 6~0.322 8 mg·mL^-1内斑蝥酸钠与峰面积的线性关系良好，平均回收率为98.9%，RSD为1.2%（n=9）。维生素B₆回归方程为Y=24.153X+0.670（r=0.999 9），在0.535 9~2.679 7 mg·mL^-1内维生素B₆与峰面积的线性关系良好，平均回收率为100.2%，RSD为1.0%（n=9）；仪器精密度、稳定性和重复性试验的RSD均<2.0%。结论 所建立的方法结果准确、重复性好，可用于斑蝥酸钠维生素B₆注射液的质量控制。     

CMIA、FPIA、MEIA与EMIT测定血药浓度的比较分析

目的：分析比较化学发光微粒子免疫分析法（CMIA）、荧光偏振免疫分析法（FPIA）、微粒子捕捉免疫分析法（MEIA）和酶扩大免疫分析法（EMIT）测定血清丙戊酸（VPA）、全血环孢霉素A（CsA）、血清卡马西平（CBZ）和血清地高辛（DIG）浓度的一致性。方法：通过测定高、中、低浓度质控样品,评价各方法的准确度及精密度,并对临床患者的VPA、CsA、CBZ和DIG样本进行测定,比较4种方法测定结果的相关性。结果：CMIA与EMIT（测定值为函数Y）比较,测定VPA的结果具有良好的相关性和差异性,Y_EMIT=1.172X_CMIA+0.227（r=0.97）,EMIT的测定结果比CMIA平均高17.49%。FPIA与EMIT比较,测定结果具有良好的相关性：VPA,Y_EMIT=1.259X_FPIA-4.671（r=0.97）;CsA,Y_EMIT=0.832X_FPIA+17.63（r=0.97）;CBZ,Y_EMIT=1.156X_FPIA-2.657（r=0.98）;MEIA与EMIT比较,测定结果有相关性：DIG,Y_EMIT=0.634X_MEIA+0.018（r=0.91）;其中CsA的EMIT测定结果比FPIA平均低2.08%,DIG的EMIT测定结果比MEIA平均低35.91%,而VPA的EMIT测定结果比FPIA平均高16.83%、CBZ的EMIT测定结果比FPIA平均高3.07%。结论：CMIA测定VPA血药浓度、FPIA测定VPA、CsA、CBZ及MEIA测定DIG血药浓度与EMIT的测定结果,存在差异性（P<0.05）,临床应用中应予以关注并作相应调整。     

HPLC法测定五味清浊散中羟基红花黄色素A的含量

摘 要 目的:建立五味清浊散中羟基红花黄色素A的高效液相色谱测定方法。方法: 色谱柱为Prevail Select C₁₈（150 mm ×4.6 mm,5 μm）,柱温35℃;流动相为乙腈-0.5% 磷酸溶液 (11∶89),流速 1 ml·min^-1;检测波长403 nm。结果:羟基红花黄色素A在16.65～166.50 μg·ml^-1范围内呈良好的线性关系,回归方程为Y=3.24×10^-2X+2.12,r=0.999 9。平均回收率为99.1%,RSD为1.9%。结论:本方法操作简便,测定结果准确可靠,可用于五味清浊散中羟基红花黄色素A的含量测定。     

Safety assessment of poloxamers 101, 105, 108, 122, 123, 124, 181, 182, 183, 184, 185, 188, 212, 215, 217, 231, 234, 235, 237, 238, 282, 284, 288, 331, 333, 334, 335, 338, 401, 402, 403, and 407, poloxamer 105 benzoate, and poloxamer 182 dibenzoate as used in cosmetics

Poloxamers are polyoxyethlyene, polyoxypropylene block polymers. The impurities of commercial grade Poloxamer 188, as an example, include low-molecular-weight substances (aldehydes and both formic and acetic acids), as well as 1,4-dioxane and residual ethylene oxide and propylene oxide. Most Poloxamers function in cosmetics as surfactants, emulsifying agents, cleansing agents, and/or solubilizing agents, and are used in 141 cosmetic products at concentrations from 0.005% to 20%. Poloxamers injected intravenously in animals are rapidly excreted in the urine, with some accumulation in lung, liver, brain, and kidney tissue. In humans, the plasma concentration of Poloxamer 188 (given intravenously) reached a maximum at 1 h, then reached a steady state. Poloxamers generally were ineffective in wound healing, but were effective in reducing postsurgical adhesions in several test systems. Poloxamers can cause hypercholesterolemia and hypertriglyceridemia in animals, but overall, they are relatively nontoxic to animals, with LD(50) values reported from 5 to 34.6 g/kg. Short-term intravenous doses up to 4 g/kg of Poloxamer 108 produced no change in body weights, but did result in diffuse hepatocellular vacuolization, renal tubular dilation in kidneys, and dose-dependent vacuolization of epithelial cells in the proximal convoluted tubules. A short-term inhalation toxicity study of Poloxamer 101 at 97 mg/m(3) identified slight alveolitis after 2 weeks of exposure, which subsided in the 2-week postexposure observation period. A short-term dermal toxicity study of Poloxamer 184 in rabbits at doses up to 1000 mg/kg produced slight erythema and slight intradermal inflammatory response on histological examination, but no dose-dependent body weight, hematology, blood chemistry, or organ weight changes. A 6-month feeding study in rats and dogs of Poloxamer 188 at exposures up to 5% in the diet produced no adverse effects. Likewise, Poloxamer 331 (tested up to 0.5 g/kg day(-1)), Poloxamer 235 (tested up to 1.0 g/kg day(-1)), and Poloxamer 338 (at 0.2 or 1.0 g/kg day(-1)) produced no adverse effects in dogs. Poloxamer 338 (at 5.0 g/kg day(-1)) produced slight transient diarrhea in dogs. Poloxamer 188 at levels up to 7.5% in diet given to rats in a 2-year feeding study produced diarrhea at 5% and 7.5% levels, a small decrease in growth at the 7.5% level, but no change in survival. Doses up to 0.5 mg/kg day(-1) for 2 years using rats produced yellow discoloration of the serum, high serum alkaline phosphatase activity, and elevated serum glutamicpyruvic transaminase and glutamic-oxalacetic transaminase activities. Poloxamers are minimal ocular irritants, but are not dermal irritants or sensitizers in animals. Data on reproductive and developmental toxicity of Poloxamers were not found. An Ames test did not identify any mutagenic activity of Poloxamer 407, with or without metabolic activation. Several studies have suggested anticarcinogenic effects of Poloxamers. Poloxamers appear to increase the sensitivity to anticancer drugs of multidrug-resistant cancer cells. In clinical testing, Poloxamer 188 increased the hydration of feces when used in combination with a bulk laxative treatment. Compared to controls, one study of angioplasty patients receiving Poloxamer 188 found a reduced myocardial infarct size and a reduced incidence of reinfarction, with no evidence of toxicity, but two other studies found no effect. Poloxamer 188 given to patients suffering from sickle cell disease had decreased pain and decreased hospitilization, compared to controls. Clinical tests of dermal irritation and sensitization were uniformly negative. The Cosmetic Ingredient Review (CIR) Expert Panel stressed that the cosmetic industry should continue to use the necessary purification procedures to keep the levels below established limits for ethylene oxide, propylene oxide, and 1,4-dioxane. The Panel did note the absence of reproductive and developmental toxicity data, but, based on molecular weight and solubility, there should be little skin penetration and any penetration of the skin should be slow. Also, the available data demonstrate that Poloxamers that are introduced into the body via routes other than dermal exposure have a rapid clearance from the body, suggesting that there would be no risk of reproductive and/or developmental toxicity. Overall, the available data do not suggest any concern about carcinogenesis. Although there are gaps in knowledge about product use, the overall information available on the types of products in which these ingredients are used, and at what concentration, indicates a pattern of use. Based on these safety test data and the information that the manufacturing process can be controlled to limit unwanted impurities, the Panel concluded that these Poloxamers are safe as used.     

HPLC法测定抗妇炎胶囊中木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱

目的 采用高效液相色谱（HPLC）法同时测定抗妇炎胶囊中木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱10种活性成分。方法 采用InerSustain AQ-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,流动相A：乙腈–无水乙醇（80∶20）,流动相B：0.1%磷酸溶液,梯度洗脱,检测波长220 nm,体积流量1.0 mL/min,柱温30℃,进样量10 μL。结果 木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱分别在2.69～134.50、1.95～97.50、0.63～31.50、0.86～43.00、11.95～597.50、0.59～29.50、6.08～304.00、4.85～242.50、1.66～83.00、19.79～989.50 μg/mL线性关系良好（r≥0.999 3）;平均回收率分别为99.11%、98.23%、96.95%、97.78%、100.02%、97.21%、99.66%、99.52%、98.81%、100.08%,RSD值分别为1.04%、1.23%、1.37%、1.65%、0.70%、1.28%、0.65%、0.81%、1.11%、0.63%。结论 建立的HPLC法可用于抗妇炎胶囊中10种活性成分的测定,作为抗妇炎胶囊质量控制方法。     

欧洲刺柏（Juniper）

活性成分与药理作用欧洲刺柏药用部位是其浆果，具有促水排泄、防腐、抗胃肠胀气和抗风湿作用，还可改善胃功能。用作促水排泄药可增加尿量（水丢失），但不增加钠排泄。成分萜品烯-4-醇可增加肾小球滤过率，但刺激肾。欧洲刺柏浆果对单纯疱疹病毒体外显示抗病毒活性，并具抗真菌活性。动物实验显示，欧洲刺柏浆果提取物具有堕胎、抗生育、抗炎、抗胚胎植入、降血压、升血压和降血糖作用。欧洲刺柏浆果油具有兴奋子宫的活性，以及利尿、胃肠道抗菌和刺激作用，该油对平滑肌有阻止解痉作用。     

Arformoterol: (R,R)-eformoterol, (R,R)-formoterol, arformoterol tartrate, eformoterol-sepracor, formoterol-sepracor, R,R-eformoterol, R,R-formoterol

Sepracor in the US is developing arformoterol [R,R-formoterol], a single isomer form of the beta(2)-adrenoceptor agonist formoterol [eformoterol]. This isomer contains two chiral centres and is being developed as an inhaled preparation for the treatment of respiratory disorders. Sepracor believes that arformoterol has the potential to be a once-daily therapy with a rapid onset of action and a duration of effect exceeding 12 hours. In 1995, Sepracor acquired New England Pharmaceuticals, a manufacturer of metered-dose and dry powder inhalers, for the purpose of preparing formulations of levosalbutamol and arformoterol. Phase II dose-ranging clinical studies of arformoterol as a longer-acting, complementary bronchodilator were completed successfully in the fourth quarter of 2000. Phase III trials of arformoterol began in September 2001. The indications for the drug appeared to be asthma and chronic obstructive pulmonary disease (COPD). However, an update of the pharmaceutical product information on the Sepracor website in September 2003 listed COPD maintenance therapy as the only indication for arformoterol. In October 2002, Sepracor stated that two pivotal phase III studies were ongoing in 1600 patients. Sepracor estimates that its NDA submission for arformoterol, which is projected for the first half of 2004, will include approximately 3000 adult subjects. Sepracor stated in July 2003 that it had completed more than 100 preclinical studies and initiated or completed 15 clinical studies for arformoterol inhalation solution for the treatment of bronchospasm in patients with COPD. In addition, Sepracor stated that the two pivotal phase III studies in 1600 patients were still progressing. In 1995, European patents were granted to Sepracor for the use of arformoterol in the treatment of asthma, and the US patent application was pending.     

Strength of drug habits: For heroin,morphine, methadone,alcohol, barbiturates,pentobarbital, benzedrine,cocaine, and marijuana

The drug habits for 78 confirmed opiate addicts were studied on eight scales from the Process Association Test of Addiction (PATA) for many drug names. Through cluster analysis eight stages of addiction were defined: “to be clean”, “to learn about drugs”, “to hustle”, “to chip” (also “to be high”), to be psychologically dependent or “to need a shot”, “to be hooked”, “to kick a habit” and “to be in treatment”. Associations stimulated by the words heroin and morphine were very similar over the eight stages of addiction in opiate addicts. The subjects were especially inclined to associate morphine and heroin with the most severe level of addiction, “to be hooked”. Associations to both methadone and cocaine were elevated at the “hooked” stage, but in other respects associations to these drugs were opposite. Thus, associations to cocaine were focused on the stage of psychological dependence and the lower intermediate stage of addiction, “to chip” and “to be high”, whereas associations to methadone suggested a turning away from addiction as indicated by avoidance associations (“to come down” and “to kick a habit”) as well as associations to “treatment” and “to be clean”. Marijuana, Benzedrine, “goofball” (barbiturates) and alcohol habits were prominent at an intermediate stage of addiction (“to chip” and “to be high”). Avoidance associations were common for Benzedrine and “goofballs” (also pentobarbital) but not for marijuana or alcohol. “Hustling” associations were frequent for marijuana but not for alcohol.