Establishment of Detection Methods for Dexamethasone Sodium Phosphate in Injections by UPLC-PDA

A detection method of dexamethasone sodium phosphate in houttuynia injection,bupleurum injection,vitamin C injection,lincomycin hydrochloride injection,and asragulus polysacharin injection was established by UPLC-PDA.The Waters ACQUITY UPLC^® BEH C18 column(2.1 mm×50 mm,1.7 μm) was used,the mobile phase consisted of 0.75% triethylamine phosphatic liquor/solution (pH 3.0)-methyl alcohol-acetonitrile(50:45:5),the flow rate was 0.3 mL/min,the column temperature had remained 25℃,photodiode array detector wavelength range was 190 to 400 nm,the recorded wavelength was 242 nm,the injection volume was 10 μL.The linear range of dexamethasone sodium phosphatel was 10.0 to 200.0 mg/L (R²=0.9999),the mean recovery and RSD for dexamethasone sodium phosphate in houttuynia injection,bupleurum injection,vitamin C injection,lincomycin hydrochloride injection and asragulus polysacharin injection were 97.54% and 1.14%,101.59% and 0.19%,100.92% and 0.92%,99.82% and 0.73%,100.08% and 0.62%,respectively.This method was accurate,easy and fast,it was suitable for detection of dexamethasone sodium phosphatein houttuynia injection and other four kinds of injections.     

Flash electroretinography in standing horses using the DTL microfiber electrode

Purpose The goal of our study was the evaluation of a practical method for the recording of flash electroretinograms (ERGs) in sedated, standing horses with the DTL? microfiber electrode. Methods The horses were sedated intravenously with detomidine hydrochloride (0.015 mg/kg). The pupil was dilated and the auriculopalpebral nerve was blocked. The ERGs were recorded with the active electrode on the cornea (DTL?), the reference electrode near the lateral canthus, and the ground electrode over the occipital bone. The light intensities of the white strobe light were 0.03 cd·s/m² (scotopic) and 3 cd·s/m² (scotopic and photopic). Photopic and scotopic single flash and flicker responses to Ganzfeld stimulation were recorded. During the 20‐min dark adaptation period the retina was stimulated every 5 min with the 0.03 cd·s/m² single flash. Results The median b‐wave amplitudes and implicit times were 38 µV and 33 ms (photopic cone‐dominated response), 43 µV and 63 ms (5‐min dark adaptation), 72 µV and 89 ms (10 min), 147 µV and 103 ms (15 min), 188 µV and 109 ms (20 min, 0.03 cd·s/m², rod response), and 186 µV and 77 ms (20 min, 3 cd·s/m², maximal combined rod‐cone response). A steady increase in amplitude and implicit time was noted during dark adaptation. No oscillatory potentials could be isolated. Conclusions The use of detomidine hydrochloride sedation and the DTL? microfiber electrode allowed the recording of good quality ERGs. This protocol should permit the detection of functional problems in the retina without the risk involved with general anesthesia.     

土霉素在鸡蛋中的残留消除研究

研究临床使用常规剂量及养殖环节加大盐酸土霉素可溶性粉剂量后其在鸡蛋中的残留消除规律。对产蛋期蛋鸡分别给予500 mg/L和667 mg/L 50%盐酸土霉素可溶性粉,集中饮水给药,每日1次,连续5 d。分别采集停药后1～12 d的鸡蛋样品,采用UPLC-MS/MS测定鸡蛋中土霉素的残留量。按上述方法给药后,低、高剂量组分别在停药第1天和停药第2天达到土霉素残留量最高。低、高剂量组的最高残留量分别为142. 72、82. 84μg/kg,均低于国家规定的最高残留限量(200μg/kg),不会造成土霉素残留超标。本试验通过研究土霉素可溶性粉在鸡蛋中的残留情况,确定弃蛋期前后土霉素残留量,以期为蛋鸡产蛋期安全用药,保障食品安全提供科学依据。     

HPLC法测定盐酸小檗碱预混剂的含量

采用HPLC法测定盐酸小檗碱预混剂中盐酸小檗碱含量。色谱柱为Agilent ZORBAXSB-C18柱(3.9mm×150mm,4μm),流动相为0.02mol/L磷酸二氢钾溶液(用磷酸调pH为2.5)-乙腈(70∶30,V/V),检测波长346nm,流速1.0mL/min,柱温为30℃,保留时间约6.2min。盐酸小檗碱浓度在5~80μg/mL范围内,峰面积与浓度呈良好的线性关系(r2=0.9999)。平均回收率99.5%,RSD为0.4%。该方法适用于检测盐酸小檗碱预混剂。     

HPLC法测定兔血清中盐酸沙拉沙星含量的研究

建立了ＨＰＬＣ（高效液相色谱）法测定兔血清中盐酸沙拉沙星的含量。固定相：色谱柱,ＨｙｐｅｒｓｉｌＣ１８柱,１０μｍ,Φ４．６＊２００ｍｍ。保护柱,ＨｙｐｅｒｓｉｌＣ１８柱,１０μｍ,Φ４．６＊３０ｍｍ。均由大连依利特科学仪器有限公司购进。流动相：０．０１％三氟乙酸－乙腈 －３％四丁基溴化铵（６０：２５：１５ｖ／ｖ／ｖ）流速：１．０ｍｌ／ｍｉｎ。保留时间３．２－３．８ｍｉｎ。灾光检测器检测波长：激发     

盐酸环丙沙星在患子宫内膜炎奶牛子宫内给药的药物浓度

本研究以反相高效液相色谱为定量分析手段，选用5头患子宫内膜炎的奶牛，通过子宫内灌注盐酸环丙沙星（2.5 g/头），研究了盐酸环丙沙星在患子宫内膜炎奶牛体内的药物动力学规律。以二氟沙星为内标，血浆样品经甲醇沉淀蛋白，离心，经针头式过滤器处理，用反相高效液相法测定其中盐酸环丙沙星的浓度。 色谱条件为：ODS-1C₁₈柱；测定流动相为0.015 mol/L四丁基溴化铵溶液-乙腈（92∶8，V/V），pH为3.0；流速为1.0 ml/min；荧光检测器，激发波长（λex）278 nm，发射波长（λem）465 nm。通过采用MCPKP房室分析程序，分析血中浓度 时间数据，发现有3头奶牛血样药时数据符合无吸收三室开放模型。其血样中主要药动学参数为：T_1/2α为0.916 h、T_1/2β为49.20 h、AUC高达7.6296 mg/L·h、Clβ为1.582 L/kg·h，β为0.642 h^-1。有2头奶牛血样药时数据符合一级吸收二室开放模型。其主要药动学参数为：T_1/2α为1.26 h、T_1/2β为9.2 h、AUC高达28.336 mg/L·h，β为0.3571 h^-1。试验结果表明，盐酸环丙沙星子宫给药吸收快，分布广，消除慢。     

高效液相色谱-串联质谱法测定猪毛中盐酸可乐定和盐酸赛庚啶

建立了高效液相色谱-串联质谱法测定猪毛中盐酸可乐定和盐酸赛庚啶的方法。猪毛样品用0.1 mol/L NaOH溶解后,用0.1 mol/L HCl溶液调节pH值至7.0,经乙腈提取后用UPLCMS/MS进行分析。分析时采用Waters BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以0.10%甲酸水/甲醇作为流动相进行梯度洗脱,电喷雾正电子(ESI~+)模式电离,多反应监测(MRM)模式检测,外标法进行定量。结果表明:盐酸可乐定和盐酸赛庚啶标准溶液在1.0~50μg/L范围内,峰面积与含量呈线性相关。盐酸可乐定和盐酸赛庚啶的检出限均为0.20μg/kg,样品中添标平均回收率在85%~110%之间,相对标准偏差(RSD)小于10%。     

High frequency of plant regeneration from anther culture in flax, Linum usitatissimum L.

The effects of induction medium compositions on flax anther culture were investigated in order to improve the efficiency of callus induction and plant regeneration. Anthers were inoculated onto the modified MS medium supplemented with five different combinations of plant growth regulators. The medium containing the combination of 2mg/l 2,4- dichlorophenoxy-acetic acid (2,4-D) and 1 mg/1 6-benzylaminopurine (BAP) produced a significantly higher number of calli forming shoots/100 responded anthers and a significant increase in overall efficiency of regeneration than the same basal medium containing 1 mg/1 a-naphthalene-acetic acid (NAA) and 2 mg/1 BAP (CK). Among the five levels of thiamin hydrochloride tested, the modified MS medium containing 10 mg/1 thiamin hydrochloride significantly increased the number of calli forming shoots/100 responded anthers and the overall efficiency of regeneration compared with the same basal medium containing 0.1 mg/1 thiamin hydrochloride. Maltose concentration had a significant effect on the percentage of anthers producing call, the number of calli forming shoots/100 responded anthers and the overall efficiency of regeneration. The medium containing 6% or 9% maltose produced the highest overall efficiency of regeneration among the five levels of maltose evaluated. Sucrose concentration significantly affected the number of calli forming shoots/100 responded anthers and the overall efficiency of regeneration, and dramatically affected the frequency of microspore-derived plants and the frequency of spontaneous chromosome doubling in microspore-derived plants. The efficiency of doubled haploid line production obtained in this study appears adequate for applied breeding programmes.     

克伦特罗残留GC-MS检测方法的建立及对自制试纸条性能的确证

建立了猪尿液中盐酸克伦特罗（CL）残留的GC-MS检测方法,并对自主研制的CL残留快速检测免疫金标试纸条（CL-Strip）进行了比较分析。结果表明,GC-MS的检测限为0.5ng/ml,CL-Strip的检测限为1.0ng/ml;CL-Strip与GC-MS两者的加标测定实验结果完全一致;用CL-Strip检测出的100份阴性尿样和18份阳性尿样,与GC-MS检测结果完全一致。说明CL-Strip与GC-MS同样灵敏、准确、稳定,由于CL-Strip具有简便、直观、快速、敏感、特异、准确等优点,建议在CL残留快速检测中推广应用。     

食品中甲醛残留量检测方法的比较

对食品中甲醛残留量的两种检测方法进行了比较研究,探讨了不同检测方法对测定结果的影响,并将试验条件进行选择,确定甲醛快速简便的检测方法。研究结果表明,盐酸苯肼法是目前测定食品中甲醛残留量较好的方法,可用于定性与定量分析。