OBJECTIVE To establish an HPLC method for the simultaneous determination of simvastatin and fenofibric acid in serum.METHODS The serum samples were centrifugalized after proteins precipitated with cyclohexane-dichlormethane(3∶1).The supernatant was evaporated to dryness by N2 and the remains were dissolved by mobile phase.It was detected by a diode array detector.The chromatographic conditions included: a Shimadzu VP-ODS analytical column(150 mm×4.6 mm) at a temperature of 25 ℃,the mobile phase consisted of methanol-water-10 % phosphoric acid(85∶14∶1) at a flow rate of 1.0 mL·min-1.Simvastatin and fenofibric acid were determined by dual wavelength,simvastatin used 238 nm,fenofibric acid used 300 nm.RESULTS The linear ranges of simvastatin and fenofibric acid were 0.20-25 mg·L-1(r=0.999 9) and 0.05-25 μg·mL-1(r=0.999 9),respectively.The average recoveries of them were 95.34 % and 91.80 %,respectively.Intra-day RSD and inter-day RSD were less than 6.4 %.CONCLUSION The method is simple,accurate and suitable for the determination of simvastatin and fenofibric acid in serum,it can be used for the study of the effects of drug combinations on pharmacokinetics,pharmacodynamics and bioequivalence.

癫痫为慢性发作性疾病~([1]),其治疗需长期预防用药,其中癫复星胶囊是治疗癫痫病的一种有效的中成药,其中含有中药远志和卡马西平等.中药远志具有安神益智、祛痰、消肿功效.

A micellar enhanced synchronous scanning-dual wavelength fluorimetric method for simultaneous determination of epinephrine,norepinephrine and dopamine has been described.After adding the sensitizing reagent,the ramifications of E,NE and DA have been respectively scanned simultaneously to examine the effect of the micellar enhanced and the factors as pH,the type and dosage of ordered medium(surfactants and cyclodextrin),reaction time,product stability,and so on which affect the intensity of systematic fluorescence.The results showed that when λ_ex was 300.0 nm,Δλ was 70.0 nm,the largest fluorescence signal of DA,which was 385.0 nm,was not disturbed in the simultaneous fluorescence spectrum gained and the mutual interference of E and NE could be eliminated by the dual-wavelength method.The largest fluorescence intensity could be got in 0.3 mol/L acetic acid-sodium acetate buffer at pH 4.6 and the heating time of E,NE and DA were 1 min,2 min and 40 min respectively.The linear ranges were 0.40～32.00 μg/L(r = 0.999 4) for epinephrine,2.45～54.00 μg/L(r = 0.999 5) for norepinephrine and 0.40～45.00 μg/L(r = 0.999 4) for dopamine.The detection limits of E,NE and DA were 0.09,0.27 and 0.08 μg/L respectively.Satisfactory results were obtained by the proposed method for determination of trace amounts of neurotransmitters in several synthetic samples.

In order to understand the concentration changes of insulin injection in clinical transtusion and guide correct clinical operation,the infusion bottle's adsorption of the insulin injection was observed and studied.In the experiment,the same processes of mixing insulin with and its transfusion as in the clinical treatment were imitated.The experiment was divided into 8 groups: glass bottles and plastic bottles.And each group was further divided into another 2 groups according to the different operation: transfusion or adsorption.By the UV spectroscopy,in the transfusion group,the insulin concentration of the sample taken after each 50 mL of the mixed solution droped was monitored.According to the different solvent,the adsorption group was divided into 3 groups: NaCl Group,50 g/L glucose group and 100 g/L glucose every 10 minutes and to detect the concentration of insulin.The results show that the group.It was shaken adsorption curve was similar between different infusion sets and different menstruums.The adsorption quantity of the plastic bottle was more than glass bottles,isotonic Na chloride was more than the glucose,the 100 g/L glucose was more than the 50 g/L glucose.Therefore the loss of adsorption should be taken into consideration in the process of clinical operation.

Synchronous scanning DW-fluorospectrophotometry was proposed for the simultaneous determination of 3 catecholamine neurotransmitters,i.e.,epinephrine(EP) norepinephrine(NEP) and dopamine(DA).It was found that satisfactory results were obtained by setting the wavelength difference(Δλ) between emission wavelength(λem) and excitation wavelength(λex) at 70 nm in the synchronous scanning fluorescence measurements.The fluorescence signals of DA measured at the λem of 385.0 nm were not interfered by EP and NEP,and the co-interference between EP and NEP was satisfactorily eliminated by adopting the mode of dual wavelength measurement.Hence,EP,NEP and DA were determined simultaneously in the same sample solution.The wavelength pairs of 470.0 nm(λem,1) and 531.8 nm(λem,2) as well as 500.0 nm(λ′em,1) and 445.6 nm(λ′em,2) were chosen for the determination of NEP and EP respectively.Linear relationships between values of fluorescence intensity and concentration of the catecholamines were found in the ranges within 320 μg·L-1(for EP),640 μg·L-1(for NEP) and 160 μg·L-1(for DA),and the detection limits(3σ/k) found were 0.20,0.97,0.73 μg·L-1 respectively.

OBJECTIVE To compare the two methods for determination of pesticide residues in the Chinese herbs. METHODS Using micellar electrokinetic chromatography(MEKC)on-line Sweeping technique and capillary gas chromatography (CGC) to determine the pesticide residues in the Chinese herbs. And the two methods sample pretreatment conditions,their detection conditions,their linear,their precision,their recovery rates,their minimum detection limit and their sample determination results were compared. RESULTS It was simple to pretreat the samples by MEKC. The MEKC has the character of wide detecting range and CGC has the advantage of low detection limit. The precision,recovery rates and the sample determination results by MEKC and CGC were not of remarkable differences. CONCLUSION MEKC and CGC had both advantages and disadvantages. CGC can not be used directly to determine non-volatile pesticide. The two method’s detection limits are lower than each country’s and both can be used to determine the pesticide residues in the Chinese herbs.

目的 通过观察麦冬细胞超声破壁时间和利用紫外分光光度法检测超声提取麦冬皂苷D含量两种考察指标来比较筛选麦冬皂苷D的提取条件,优化超声提取工艺.方法 采用正交设计法,分别以麦冬细胞破壁时间和采用紫外分光光度法测定麦冬细胞破壁后皂苷D的含量为考察指标,考察乙醇浓度、温度、麦冬粒度和先期浸泡时间等因素对超声提取工艺的影响.通过显微镜观察,确定细胞破壁状况;通过对两种考察指标的实验结果 进行比较,优化提取方案.结果 利用紫外分光光度法测定麦冬皂苷D含量和通过观察麦冬细胞破壁所筛选的麦冬皂苷D最佳提取工艺的结果 是一致的.在考察因素中,麦冬皂苷提取工艺影响程度为:粒度﹥乙醇浓度﹥先期浸泡时间﹥温度,超声提取最佳条件为:温度45 ℃,80 目粒度,95% 乙醇,先期浸泡12 h.结论 通过超声方法 对中草药有效成分进行提取,其提取率与细胞破壁有关,利用正交实验分析紫外分光光度法检测麦冬皂苷D含量和考察麦冬细胞破碎的结果 是一致的,可通过观察麦冬细胞破壁结果 来优化提取工艺,简化操作.

胶束毛细管电泳在分离科学中的应用已有广泛报道,但因其检测灵敏度不高,故其在痕量分析中的应用受到一定限制.

Objective:A micellar electrokinetie chromatography (MEKC) method based on on-line sweeping tech- nique was developed for determination of trace acetamiprid and imidacloprid in traditional Chinese medicines. Methods:The traditional Chinese medicines samples,to which some methanol was first added,were extracted by ul- trasonic,and leached by dichloromethane and in the running buffer of 20 mmol·L~(-1) Na_2B_4O_7+80 mmol·L~(-1) so- dium dodecyl sulfate(SDS),pH = 6.93,the acetamiprid and imidacloprid in samples were successfully separated and detected within 100 s,in a non-coating fused-silica capillary column(48.5 cm× 50 μm i.d.,effective length 40 cm)at separation voltage of 15 kV,and the injection pressure of 4.5 kPa,with UV detection at 262 nm. Results:The detection limits of acetamiprid and imidacloprid were 0.008 mg·kg~(-1) and 0.016 mg·kg~(-1),respec- tively.This method allows of up to 270-and 210-fold accumulation concentration of acetamiprid and imidaclo- prid.Conclusions:This method can make the pretreatment of the traditional Chinese medicine samples simple and the detection limits are low.It can he used to separate and determine the trace pesticide residuals of acetamiprid and imidacloprid in traditional Chinese medicines.

To determine acetamiprid pesticide residue in the Chinese herbs by capillary gas chromatography with electron capture detector(CGC-ECD).Samples were extracted with methanol solvent by ultrasonic,then cleaned up by a column packed with Florisil.The capillary column was DB-1(30 m×0.25 mm×0.25 μm); the column temperature program: initial 180 ℃(hold 2 min),rate of 10 ℃/min to 250 ℃.The pesticide residue had good linear correlation within 6.70×10-4～1.50 mg/L,the limit of detection was 6.0×10-4 mg/L,and the lowest quality of detection was 6.0×10-10 mg.All of samples were detected to have acetamiprid pesticide residue.The method has low detection limit,good purification effection and repeatability.It can be used to determine the trace pesticide residual of acetamiprid in the Chinese herbs.

OBJECTIVE To observe the changes of insulin concentration in clinical transfusion and the adsorption quantity in different infusion sets.METHODS In the experiment,the same processes of mixing insulin and its transfusion as in the clinical treatment were imitated.The experiment was divided into 18 groups: isotonic Na chloride(glass bottles and plastic bottles),5% glucose injection(glass bottles and plastic bottles) and 10% glucose injection(glass bottles and plastic bottles),each group was further divided into another 3 groups according to the different operation: The first group was shaken regularly in the process of transfusion the second group was not shaken at all let it transfused naturally.Insulin concentration of the sample taken after each 50 mL of the mixed solution droped was monitored by UV Spectrophotometry.The third group was shaken every 10 minutes and to detect the concentration of insulin.RESULTS The insulin concentration of the glass bottles groups,compared with that of the plastic bottle groups had no obvious differences,but there were some difference between the different injections.The insulin concentration of the natural dropping groups increased suddenly,but became stable when the transfusion set was shaken properly.The adsorption curve was similar between different infusion sets and different menstruum.The adsorption quantity of the plastic bottle was more than glass bottles isotonic Na chloride was more than the glucose.CONCLUSION The proper shaking of the transfusion set in the process of transfusion of insulin can effectually avoid the increase of insulin concentration in the procedure of transfusion to prevent the hypoglycemia.

A synchronous scanning-dual wavelength fluorimetric method for simultaneous determination of epinephrine, norepinephrine and dopamine has been described. The ramifications of Einverted commas NE and DA have been respectively scanned simultaneously to examine the factors which affect the intensity of systematic fluorescence. When Δλ was 70 nm, the largest fluorescence signal of DA, which was 385 nm, was not disturbed in the simultaneous fluorescence spectrum gained and the mutual interference of E and NE could be eliminated by the dual-wavelength method. The largest fluorescence intensity could be got in 0.5 mol·L-1 acetic acid sodium acetate buffer at pH 6.5 and the heating time of E, NE and DA were 1 min, 3 min and 35 min respectively. The linear ranges were 1-320 ng·mL-1 (r = 0.9995) for epinephrine, 3-640 ng·mL-1 (r = 0.9998) for norepinephrine and 1-160 ng·mL (r = 0.9993) for dopamine. The detection limits of E, NE and DA were 0.20 ng·mL-1, 0.97 ng·mL-1 and 0.73 ng·mL-1 respectively. Satisfactory results were obtained by the proposed method for determination of trace amounts of neurotransmitters in several synthetic samples.