微波消解-ICP-MS法同时测定食品用纸容器中15种元素

建立了电感耦合等离子体质谱(ICP-MS)结合微波消解测定食品用纸容器中15种元素的方法。试样经硝酸-过氧化氢混合溶液微波消解,ICP-MS测定,外标法定量。回收率在90%~120%之间,相对标准偏差均小于5%。该方法操作简便、灵敏度高,具有消解速度快、污染小、样品消解完全、回收率高的特点,适用于食品用纸容器中15种元素的同时分析。     

气相色谱法测定复方水合氯醛口服溶液中水合氯醛含量

目的:采用气相色谱建立复方水合氯醛口服溶液中水合氯醛的含量测定方法。方法:色谱柱:OV-624毛细管柱(30m×0. 53 mm,0. 5μm);柱温:100℃;氢离子火焰检测器(FID)温度:250℃;进样口温度:200℃;载气压力:氮气50 k Pa;氢气50 k Pa;空气流量:40 m L/min;进样量:1μL,进样方式:分流进样(1∶100);在此条件下进行方法学考察。结果:测定复方水合氯醛口服溶液中水合氯醛含量时,各方法学参数满足《中国药典》要求,水合氯醛在125μg/m L～2000μg/m L呈良好线性关系,精密度、重复性RSD分别为1. 96%、2. 97%;样品平均回收率为101. 04%,RSD为2. 03%。结论:气相色谱法适用于复方水合氯醛口服溶液中水合氯醛含量测定,且操作方便,简单易行。     

微波等离子体光谱仪(MP-AES)高效测定啤酒中15种元素的方法研究

本文主要研究了微波等离子体原子发射光谱仪(MP-AES)同时测定精酿啤酒中的镉(Cd)、锌(Zn)、钴(Co)、镍(Ni)、锰(Mn)、铝(Al)、铜(Cu)、锶(Sr)、钼(Mo)、钾(K)、铬(Cr)、铅(Pb)、钡(Ba)、硒(Se)、砷(As) 15种元素的可行性。各种元素标准曲线线性良好,检出限在0.003～0.56 mg/L之间,相关系数不小于0.999,相对标准偏差在1.8%以内,15种元素方法回收率80.0%～120%。各元素的测定结果表明,该方法简单、快速、灵敏度高、线性范围宽、可操作性强,可同时测定啤酒中15种元素,并且无需使用任何易燃的危险气体(乙炔、一氧化二氮)或昂贵的稀有气体(氩气),较之传统原子吸收光谱法(AAS)具有诸多优势。     

复方氨酚右敏溶液在健康人体的药代动力学研究

研究复方氨酚右敏溶液在健康人体的药代动力学.12名健康受试者以自身为对照采用随机交叉给药方式,单次空腹口服3个剂量复方氨酚右敏溶液(低、中、高3个剂量分别为7.5、15、30 mL,每mL含对乙酰氨基酚32 mg、马来酸右氯苯那敏0.1 mg).用液相色谱-串联质谱法(LC-MS/MS)测定血浆中对乙酰氨基酚和马来酸右氯苯那敏的浓度,计算2种药物的药代动力学参数,评价其药代动力学特征.对乙酰氨基酚在人体内的动力学过程符合二室模型,低、中、高3个剂量主要药代动力学参数消除半衰期t1/2分别为(2.93±0.47)、(3.08±0.43)、(3.01±0.49) h,血药质量浓度时间曲线下面积AUC0～t分别为(12.29±3.91)、(27.80±7.64)、(60.41±17.24) μg·h·mL-1;右氯苯那敏在人体内的动力学过程符合一室模型,低、中、高3个剂量主要药代动力学t1/2分别为(20.49±7.86)、(19.66±5.05)、(19.96±6.48) h;AUC0～t分别为(32.61±13.65)、(67.58±23.31)、(158.12±56.44) ng·h·mL-1.对乙酰氨基酚和右氯苯那敏药动学参数ρmax、AUC0～t、AUC0～∞均与给药剂量呈线性相关(P<0.001),复方氨酚右敏溶液在7.5～30 mL剂量范围内呈线性人体药代动力学特征.     

反相高效液相色谱法测定牙膏中的甘草次酸

采用反相高效液相色谱法测定了牙膏中的甘草次酸.在YWG-C18(1.0mmi.d.×250 mm,10 μm)色谱柱上,以甲醛0.01 mol/L KH2PO4=8515(VV,pH3.0)的溶液为流动相,流速为1.0 mL/min,紫外检测波长为254nm,室温下检测.甘草次酸用甲醇提取.甘草次酸的平均回收率为99.61%～101.67%,方法的相对标准偏差为1.85%～3.16%.方法操作简便、快速和准确.     

HPLC法测定复方珊瑚姜溶液尿素咪康唑软膏复合制剂中硝酸咪康唑含量

通过采用十八烷基硅烷键合硅胶为填充剂的色谱柱,以甲醇-0.35%磷酸溶液(用三乙胺调pH至3.2)(80∶20)为流动相,流速1.0 mL/min,检测波长为230 nm,柱温25℃,进样量为10μL,建立复方珊瑚姜溶液尿素咪康唑软膏复合制剂中硝酸咪康唑含量测定的方法。结果表明:硝酸咪康唑在0.049 90～0.848 3μg范围内线性关系良好(r=1.000),方法回收率为97.13%(n=9,RSD=0.56%)。建立的方法简便、快速、准确及可靠,可用于复方珊瑚姜溶液尿素咪康唑软膏复合制剂中硝酸咪康唑的定量测定。     

甘草及复方甘草片核磁共振氢谱的研究

采用核磁共振波谱仪测定了两种不同产地的甘草及三种不同厂家生产的复方甘草片乙醇提取物的核磁共振氢谱图谱。分析结果显示,甘草及复方甘草片均出现其代表性化学成分的特征共振峰,甘草及复方甘草片的核磁共振氢谱可用做甘草及复方甘草片的鉴别依据。     

甘草及复方甘草片核磁共振氢谱的研究

采用核磁共振波谱仪测定了两种不同产地的甘草及三种不同厂家生产的复方甘草片乙醇提取物的核磁共振氢谱图谱.分析结果显示,甘草及复方甘草片均出现其代表性化学成分的特征共振峰,甘草及复方甘草片的核磁共振氢谱可用做甘草及复方甘草片的鉴别依据.     

微波消解-ICP-AES法测定大米和小麦粉中21种无机元素

以电感耦合等离子体原子发射光谱法(ICP-AES)测定山西大同大学食堂大米和小麦粉中21种无机元素的含量。该方法测定各元素的相关系数在0.995 0～0.999 9之间,仪器检出限在0.000 4～0.103 8μg/mL之间,选取Mn,Ca,Mg,K做加标回收实验,回收率在91.57%～105.60%之间,相对标准偏差(RSD)在0.54%～2.50%之间(测定次数n=3),方法快速、准确、可靠。检测发现,所测大米和小麦粉中均含K,Ca,Na,Mg,Fe,Mn,Cu,Zn,Cr,B,P,Si,Li和Se等人体必需的矿质元素;均未检测到Cd,Pb,Co,Ni以及有毒元素Hg和As,但均检测到Al元素,摄入过量会影响Fe,Ca元素的吸收。     

亚临界水萃取甘草残渣共提取甘草总黄酮及低聚糖

以甘草残渣为原料,开展亚临界水萃取(SWE)甘草总黄酮及低聚糖的研究。由木质纤维素含量的测定及高效液相色谱仪(HPLC)检测结果表明:在亚临界水萃取甘草总黄酮过程中,甘草残渣中的木质纤维素存在溶出现象,且以半纤维素为主,并伴随低聚糖的生成;升高温度可促进木质纤维素解聚,从而提高甘草总黄酮和低聚糖的提取率,但长时间高温萃取会造成甘草总黄酮的降解和低聚糖的分解,并加速了木质素的溶出,对提取形成阻碍。通过正交设计优化的萃取条件为甘草残渣粒径250～425μm、液固比15 mL/g、185℃萃取135 min。在此萃取条件下,甘草总黄酮提取率为2.81%,低聚糖提取率为9.6%(其中81.3%为低聚木糖)。该研究表明亚临界水萃取可实现甘草总黄酮与低聚糖的共提取。     

Determination of ciprofloxacin hydrochloride in pharmaceutical preparation and biological fluid by Rayleigh light scattering technique

A highly sensitive and simple Rayleigh light scattering (RLS) method for determination of ciprofloxacin hydrochloride has been developed. Ciprofloxacin hydrochloride (CPFH) reacted with tetraphenylboron sodium(TPB) to form an ion-association complex in pH 5.31 aqueous solution, which resulted in a significant enhancement of the RLS intensity, which was linear with the concentration of CPFH in the range of 12.7–419 ng·mL⁻¹. The limit of detection for CPFH was 6.99 ng·mL⁻¹. The method is simple, highly sensitive and selective within a wide linear range. Appliying this method to determination of ciprofloxacin hydrochloride in pharmaceutical preparations and biological fluids obtained satisfactory results. Foundation item: Supported by the National Natural Science Foundation of China(20675059) and Research Foundation of Leshan Teachers’ College, China (Z0625)     

Spectrofluorimetric determination of magnesium (II) with 7-(8-Hydroxy-3, 6-disulfonaphthylazo)-8-hydroxyquinoline-5-sulfonic acid

A new fluorescent reagent, 7-(8-hydroxy-3, 6-disulfonaphthylazo)-8-hydroxyquinoline-5-sulfonic acid (HDNHQ) for the determination of magnesium has been developed. It reacted with magnesium to form a 1∶1 fluorescent complex withλ _ex/λ _em immediately at room temperature in ammonia-ammonium chloride buffer (pH 10.7). A linear relationship was obtained in the magnesium concentration range of 0–160 ng·mL⁻¹ with the detection limit of 0.04 ng·mL⁻¹. The proposed method was simple, rapid and sensitive. It has been successfully applied to the determination of trace magnesium in blood serum with recoveries of 103.75% and 98.16%, respectively. Foundation item: Supported by the Zi-Qiang Foundation of Wuhan University Biography: Zhang Xian (1975-), female, Ph. D candidant, research direction: organic reagent synthesis and analysis.     

基于反应体系的表面增强拉曼光谱快速检测乙基麦芽酚

以铁离子(Fe~(3+))为媒介,鞣酸还原氯金酸制备的金纳米粒子(Au NPs)作为表面增强拉曼散射(SERS)基底,实现比色-散射光谱双响应,快速鉴别食品中的乙基麦芽酚.其中比色法中,对乙基麦芽酚的检测限为0.50 mg·mL~(-1).SERS检测中,利用Fe~(3+)和乙基麦芽酚的络合作用,乙基麦芽酚的最低检测限降低到0.01 mg·mL~(-1),线性范围为0.05～1.00 mg·mL~(-1).该方法使用的仪器简单,操作方便,可对样品中的乙基麦芽酚进行现场直接测定.     

Flow-injection microcolumn on-line preconcentration for the determination of chromium (VI)

A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast adsorption of chromium (VI) on the high surface area nanometer-size TiO₂ (anatase) powders, which prepared by a sol-gel method from hydrolysis of TiCl₄ and (ii) the quantitative and reproducible elution of Cr (VI) by 2.0 mol·L⁻¹ HCl. A mini-column system for preconcentration is developed, Cr(VI) on the mini-column is eluted and merged with a stream water and DPCB (1,5-diphenylcarbazide) as the chromogenic reagent. The proposed system permits throughputs of 6 sample h⁻¹ (0.001 μg·mL⁻¹ Cr(VI)) or 20 sample h⁻¹ (0.1 μg·mL⁻¹ Cr(VI)). The preconcentration factor is 55. The detection limit is 0.8 ng · mL⁻¹ Cr(VI). The reproducibility is satisfactory with a relative standard deviation of less than 3.35% (0.01 μg·mL⁻¹ Cr(VI),n=5). Supported by the National Natural Science Foundation of China Ma Wanhong: born in 1961, Ph. D. Graduate student, Associate professor     

Sensitive Determination of DNA by RLS Enhancement of Metal Ions

0　IntroductionThequantitativeanalysisofnucleicacids,especiallythemi cro determinationofnucleicacids,isbecomingmoreandmoreimportantinmanybiologicalstudies.Recently ,apromisingspectraltechnique ,whichwasbasedonthemeasurementofen hancedresonancelightscattering (RLS) [1 ,2 ] ,hasgivenrisetostronginterestbyanalystsandbiochemistsfornucleicacidsandproteinassay[3 9] .Uptonow ,manykindscompoundshavebeenfoundRLSenhancementwhilebindingtoDNA ,andallthesecompoundsarecharacterizedofpositivechargewhicha…     

药物中半胱氨酸的流动注射荧光测定方法研究

 在近中性介质及聚乙烯醇(PVA)存在下,半胱氨酸能熄灭一个新的荧光试剂5-(4-氯苯基)-8-苯磺酰氨基喹啉(CPBSQ)与Cu(Ⅱ)络合体系的荧光的反应.基于此现象,本文建立了一个测定半胱氨酸的流动注射荧光熄灭方法.结果表明,在λ_ex/λ_em=327/368nm处测定,方法的进样频率为64h-1,检测范围为0.05～5.5μg·mL^-1,检出下限为0.01μg·mL^-1,对4.0μg·mL^-1半胱氨酸平行测定11次的相对标准偏差为1.52%.大量存在的常见金属离子、蛋白质及很多不带巯基的氨基酸不干扰测定.应用此方法测定了某些注射液针剂中半胱氨酸的含量,结果满意.     

反相高效液相色谱法测定维生素K2(20)

 采用外标法测定维生素K₂(20)的含量,建立了维生素K₂(20)的RP-HPLC测定方法.色谱柱为Agilent ZORBAX Eclipse XDB-C18(150 mm×Φ4.6 mm,5μm),流动相为甲醇,检测波长为270 nm,流速为1.0mL·min^-1,线性范围为0.04~0.4 mg·mL^-1(r=0.999 6).方法操作简便,重现性好,可用于维生素K₂(20)的含量测定.     

Photodegradation of bisphenol a induced by metal ions in aqueous solution in the presence of ascorbic acid

The photodegradation of bisphenol A (BPA) in aqueous solution containing metal ions and ascorbic acid (AsA) was investigated. After strong irradiation, the aqueous solution containing AsA and Cu²⁺ could produce hydroxyl radicals that induced the photodegradation of BPA. The photodegradation efficiency of BPA in the solution containing 70 μmol·L⁻¹ Cu²⁺ and 15 mg·L⁻¹ AsA reached 59% at pH 6.0 after 4 hours irradiation with high pressure mercury lamp. The photodegradation efficiency of BPA reached 10% after 4 hours irradiation with daylight lamp in the presence of 70 μmol·L⁻¹ Cu²⁺ and 15 mg·L⁻¹ ascorbic acid. BPA was not degraded in the aqueous solution only containing AsA or Cu²⁺. The BPA photodegradation in aqueous solution containing AsA and Fe³⁺ was weaker than in aqueous solution that containing AsA and Cu²⁺ at the same concentration. This work showed a new route of the BPA photodegradation in aqueous environment. Biography: PENG Zhang’e (1970–), female, Ph. D. candidate, research direction: aquatic environmental chemistry.     

Characteristics of Baicalin Synergy with Penicillin or Notopterygium Ethanol Extracts Against Staphylococcus aureus

Introduction Staphylococcus aureus (S. aureus) resistance to most once powerful β-lactame antibiotics is now a severe problem world wide, so agents are urgently needed to reduce or moderate resistance to existing antibiotics. Traditional medicinal herbs …     

催化H2O2氧化吖啶黄固体基质室温磷光法测定痕量秋水仙碱

基于秋水仙碱(COL)能催化过氧化氢(H_2O_2)氧化吖啶黄(AY)的反应,导致AY的室温磷光信号(RTP)剧烈猝灭,据此建立了超灵敏催化H2O2氧化AY固体基质室温磷光法(SS-RTP)测定COL的新方法。此方法的量化限(LOQ)为0.12 fg/斑(对应浓度为3.1×10–13 g·m L–1),灵敏度高、简便、快捷、准确。用于血清中COL的测定,结果与UPLC-MS/MS相吻合。同时测定了动力学常数,其活化能(E)为40.53 k J·mol~(–1),速度反应常数(k)为3.97×10~(–4)·s~(–1)。