Quality Control of Tramadol in Kisangani: Development, Validation, and Application of a UV-Vis Spectroscopic Method

Context: Substandard and falsified medicines are circulating in low-income countries mostly without any control. We availed a simple and not expensive UV-Vis spectroscopic method to evaluate the quality of tramadol in Kisangani before and during the Covid-19 period. Methods: For the analytical quantitative method, an experimental design was applied to set up the optimal levels of the selected factors, namely, pH of dissolution medium, type of cuvette, and wavelength. Taking into account the capsule pharmaceutical formulation within 80 - 120 μg·mL-1 concentration range, we analyzed 89 tramadol samples from pharmacies and hospitals of the six Kisangani municipalities. Results: pH showed a significant effect on absorbance, whereas quartz cuvette and wavelength did not. A typical 100 μg·mL-1 tramadol solution gave an absorbance of 0.64 at 272 nm. Validation highlighted a matrix effect observed with a 6% bias. A correction factor of 0.9372 allowed to improve the accuracy profile, which were then totally included within the 10% acceptance limits. Quality control revealed that 25 samples out of 89 were not compliant in terms of manufacturing license, registration status in DRC and content as well. Conclusion: This study showed that the strengthening of analytical strategy in Kisangani is a need.

Estimating Aluminum Leaching into Meat Baked with Aluminum Foil Using Gravimetric and UV-Vis Spectrophotometric Method

Baking meat by wrapping them in Aluminum (Al) foil is common in many countries. The excessive use of Al foil in baking and the disagreement about using Al foils were the motivation to do this study especially after the 2007 WHO/FDA Report. In this investigation, a gravimetric and a UV-Vis spectrophotometric method are used to estimate Aluminum (Al) leaching into meat baked by wrapping in Al foil. Three kinds of meat were used fish, cow stakes and chicken. The importance of Al exposure area was neglected by many studies. Five factors affecting Al leaching into meat are studied (baking temperature, baking time, additives, Al exposure area and weight of meat). The effect of cooking times (20, 40, 60 minutes) at 180℃ and cooking temperatures (160℃, 180℃, 200℃) at 60 minutes on the amount of Al leaching were evaluated. It was found that Al leaching into meat increased with increasing temperature, baking time, additives and Al exposure area. Moreover, Al exposure area was more effective than the weight of the meat. The Al leaching was highest in fish and lowest in chicken. Comparing the present results with the Provisional Tolerance Weekly Intake of Al approved by WHO/FDA, it shows that Al leaching into meat baked by wrapping in Al foil may add considerable doses into the diet. Continuous monitoring of Al foil used for baking meat is recommended.

UV-VIS分光光度法在环境监测上的应用及测定方法的选择

近三年来,国家环境保护部修订或更新了许多用UV-VIS(紫外-可见)分光光度法测定环境指标的标准方法。就UV-VIS分光光度法在环境监测领域中的应用进行分类阐述,并对环境指标的测定方法选择进行分析。

The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

Development of an analytical method for multi-residue quantification of 18 anthelmintics in various animal-based food products using liquid chromatography-tandem mass spectrometry

In this study,we developed a simple screening procedure for the determination of 18 anthelmintics(including benzimidazoles,macrocyclic lactones,salicylanilides,substituted phenols,tetrahydropyrimidines,and imidazothiazoles)in five animal-derived food matrices(chicken muscle,pork,beef,milk,and egg)using liquid chromatography-tandem mass spectrometry.Analytes were extracted using acetonitrile/1% acetic acid(milk and egg)and acetonitrile/1% acetic acid with 0.5 mL of distilled water(chicken muscle,pork,and beef),and purified using saturated n-hexane/acetonitrile.A reversed-phase analytical column and a mobile phase consisting of(A)10 mM ammonium formate in distilled water and(B)methanol were used to achieve optimal chromatographic separation.Matrix-matched standard calibration curves(R^(2)≥0.9752)were obtained for concentration equivalent to ×1/2,×1,×2,×3,×4,and×5 fold the maximum residue limit(MRL)stipulated by the Korean Ministry of Food and Drug Safety.Recoveries of 61.2e118.4%,with relative standard deviations(RSDs)of ≤19.9%(intraday and interday),were obtained for each sample at three spiking concentrations(×1/2,×1,and ×2 the MRL values).Limits of detection,limits of quantification,and matrix effects were 0.02e5.5 mg/kg,0.06e10 mg/kg,and -98.8 to 13.9%(at 20 μg/kg),respectively.In five samples of each food matrix(chicken muscle,pork,beef,milk,and egg)purchased from large retailers in Seoul that were tested,none of the target analytes were detected.It has therefore been shown that this protocol is adaptable,accurate,and precise for the quantification of anthelmintic residues in foods of animal origin.

Study on Monoxide Emission Spectrometry of Rare Earth Elements Ⅰ. Determination of Sm in Rare Earth Concentrate by Dual Wavelength Method

On the basis of investigated enhancement effect of La, Nd, Eu, and Y on Sm determination with monoxide molecular emission spectrometry, La was selected as enhancement agent and chemical interference inhibitor. In the presence of La, dual wavelength mothod was introduced to eliminate the spectral interference on Sm by other elements. A new method was established to determine samarium in high yttrium rare earth samples with satisfactory results.

A novel sample preparation method of matrix-assisted laser desorption/ionization time of flight mass spectrometry for polystyrene

A novel sample preparation method of matrix-assisted laser desorption/ionization mass spectrometry for polystyrene was reported. Compared to the conventional dried-droplet method, the efficiency of ionization and signal intensity of mass spectra were improved. The mechanism was also analyzed.

Effects of Different Pretreatment Methods on Determination of Microelements in Feed

[ Objective] To study the effects of different pretreatment methods on determination of microelement in feed and thus find the best pre treatment method for each microetement, t Method] The samples （concentrated feeding stuff and fodder） were pretreated through throe methods, that is, dry incineration method, HNOs HCIO, wetdecomposition method and microwave digestion method. Then the content of seven kinds of mi croelement （AI, Ca, Cu, Fe, Mn, Se and Zn） was determined by inductively coupled plasma atomic emission spectrometer （ICPAES）. I Result] These three methods were all suitable for the determination of Cu, Mn and Zn in concentrated feeding stuff and the determination of Cu and Ca in fodder. The content of Cu and Ca was higher in fodder detected by HNO3 HCIO, wetdecomposition method. The microwave digestion method was suitable for the determination of AI and Ca in concentrated feeding stuff and the determination of AI, Fe, Mn and Zn in fodder. The dry incinera tion method was fit for the determination of Fe in concentrated feeding stuff. [ Condusionl The content of different microelements should be deter mined after the feed is treated with different Ioretreatment methods.

解冻方式对新疆干辣椒炒牛肉预制菜品质的影响

为探究解冻方式对新疆干辣椒炒牛肉预制菜品质的影响,本研究选取自然解冻、流水解冻、超声波解冻、微波解冻和低温解冻作为解冻方式,分析5种解冻方式对新疆干辣椒炒牛肉预制菜pH值、色泽、质构特性、挥发性盐基氮(TVB-N值)、硫代巴比妥酸值(TBARS值)和挥发性风味物质品质指标的影响。结果表明,与空白对照组相比,低温解冻在维持新疆干辣椒炒牛肉预制菜pH值(5.19)和色泽方面表现最佳,超声波解冻的质构特性最好且TVB-N值最低(7.35 mg·100 g^(-1)),微波解冻的TBARS值最低(0.36 mg·kg^(-1)),微波解冻和低温解冻后新疆干辣椒炒牛肉预制菜的感官评分较好,流水解冻各项指标处于中间位置。D-柠檬烯、苯甲醛、苯乙醛、壬醛、芳樟醇、苯乙醇、α-松油醇、3-甲基-苯酚、萘、茴香脑、草蒿脑等挥发性风味物质对新疆干辣椒炒牛肉预制菜总体风味的形成有重要贡献,低温解冻后的挥发性风味物质最接近空白对照组。本研究可为新疆干辣椒炒牛肉预制菜的解冻工艺提供支撑。

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

A An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of 24 elements （Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb） in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

MALDI-TOF Mass Spectrometry Study of the Phosphorylated Tau Peptides

Fragmentation of phosphorylated Tau peptides in matrix assisted laser desorption-/ionization-time of flight-mass spectrometry (MALDI-TOF-MS) has been investigated. According to the post-source decay (PSD) in MALDI-TOF-MS, there are two different patterns of cleavage in phosphopeptides, which can be used to determine the phosphorylated site in peptides. In the synthetic tau peptides, the fragmentation at proline residue occurs strongly and this is useful to determine the structure of tau peptides.

Rapid quantification of the metabolite of valacyclovir hydrochloride in human plasma by liquid chromatography-tandem mass spectrometry

Objective To establish a rapid,sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of acyclovir (the metabolite of valacyclovir hydrochloride) in human plasma. Methods After addition of ganciclovir as internal standard (IS),plasma samples were prepared by one-step protein precipitation using acetonitrile as precipitant,followed by an isocratic elution with 0.1% formic acid solution-methanol (95∶5,v/v) on an Agilent ZORBAX SB-C18 (150mm×2.1mm i.d.,3.5μm) column. Detection was performed on a triple-quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operating in positive ion and selected reaction monitoring (SRM) mode with the precursor to product ion transitions m/z 226.2→152.1 for acyclovir and m/z 256.2→152.1 for the IS. Results The analytical results demonstrated a good linearity over the ranges from 0.005 to 4μg/mL (r=0.9999) for valacyclovir hydrochloride. The relative standard deviations (RSD) of intra-batch and inter-batch were less than 4.06% and 9.23%,respectively. The limit of detection and lower limit of quantification in human plasma were 2ng/mL and 5ng/mL,respectively. Conclusion The method was simple,sensitive,accurate and reproducible and has been successfully applied to a bioequivalence study of valacyclovir hydrochloride capsules in Chinese healthy male volunteers.

Determination of Utratrace Silver Using Surfactant As Sensitizer by Catalytic Near Field Laser Thermal Lens Spectrometry

A new method for the determination of utratrace silver(I) by near field thermal lens spectrometry has been developed. This method is based on the silver(I) catalyzed discoloring reaction of bromocresol green oxidized by sodium persulphate in the presence of a, a-bipy as activator and Triton X-100 as sensitizer. The linear range of this method is 0~1.6 ng穖L-1 of silver. The detection limit is 2?0-2 ng穖L-1. The method has been applied to the determination of silver in lead power and photographic paper with satisfactory results.

The Preparation of Nano Silver by Chemical Reduction Method

A silver nanostructures prepared by using chemical reduction method. The silver nanoparticles were prepared with diameters of about (20 nm). Numerous techniques had been used to study the optical, structural like the UV-Vis absorption spectrometer, Ttransmission Electron Microscopy (TEM), Field-Emission Scanning Electron microscope (FESEM), and X-ray diffraction (XRD). The practical results exhibited the absorption spectrum of the prepared nanoparticles at (357 nm), it was found that there is a relationship between the positions of the optical absorption peak and the size of the silver nanoparticles. The analysis of TEM results showed the presence of nanoparticles in the range (20 nm). The analyzing of XRD results explained the crystal structure for silver nanoparticles. It is found a cubic unit cell have a lattice constants (a = 4.0855 Å), with the Miller indices were (111), (002), (002), and (113).

Quantification of Phases in Lahore (Pakistan) Airborne Particulates by Matrix-Flushing Method

The mass concentrations of eighteen airborne samples collected from Lahore (Pakistan) are found in the range from 595 to 3027μg/m3with average value of 1130 μg/m3. Most of these values are normal and as reported in the literature for other parts of the world. The major phases identified in the samples by the X-ray powder diffraction technique are Albite (Anorthite), Calcite, Clinochlore (Chlorite), Gypsum, Illite, Quartz and Talc which have also been reported by other researchers to be present in the airborne particulates of other world locations. The average weight percentages of the phases (minerals) in the samples are respectively 15.5, 10.6, 23.7, 2.4, 19.1, 20.2, and 8.5. Some of the elements (e.g., boron, cadmium, lithium, manganese, titanium, and zinc) quantified in two samples determined using a spark-source mass spectrometer appear also to derive their origin from man-made activities. However no compound synthesized in the atmosphere is detected by the X-ray diffraction method.

干燥方式对苹果干品质特性及风味的影响

为探究提高静宁苹果干零食品质的加工方式,本研究探讨了5种干燥方式(热风干燥、太阳能干燥、真空冷冻干燥、微波-压差膨化干燥和热泵干燥)对苹果干能耗、抗氧化活性、微观结构和风味的影响。结果表明,和其它4种方式相比,在能耗方面,真空冷冻干燥的单位能耗最高(69.48±1.69 kW·h/kg),而太阳能干燥的单位能耗最低(19.60±1.36 kW·h/kg);在硬脆度方面,热风干燥的苹果干具有最高的硬度、最低的脆度,而真空冷冻干燥的苹果干硬度最低、脆度较高;在色差方面,真空冷冻干燥苹果干的L*值最高(72.91±0.59),ΔE值最接近鲜样(10.48±0.30);此外,真空冷冻干燥能有效降低苹果干中抗氧化物质的损失,与鲜样相比,其抗坏血酸、总酚和总黄酮的含量分别降低了35.22%、39.27%和32.02%。同时,总抗氧化能力、羟自由基清除率和超氧阴离子清除率也分别降低了23.50%、57.24%和10.56%;在微观结构方面,真空冷冻干燥的苹果干细胞层呈较规律的海绵状多孔性结构,质地较好;在风味方面,鉴定出5种干燥方式的苹果干有96种挥发性物质,其中真空冷冻干燥的苹果干更加芳香、口感更加丰富。综合考虑,真空冷冻干燥是提高苹果干零食品质特性和风味的推荐方法,对苹果干制品的工业化生产有现实的指导意义。

基于GC-IMS和GC-MS技术结合化学计量法分析干燥方式对香椿挥发性成分的影响

为研究干燥方式对香椿挥发性风味物质的影响,利用气相色谱-离子迁移谱技术(gaschromatography-ion mobility spectrometry,GC-IMS)和气相色谱-质谱联用技术(gas chromatography-mass spectrometry,GC-MS)、相对香气活性值(relative odor activity value,ROAV)对真空冷冻干燥、热泵干燥、热风干燥、微波真空干燥的香椿样品进行挥发性成分分析,并进一步结合化学计量方法主成分分析(principal component analysis,PCA)和偏最小二乘判别分析(partial least squares-discriminant analysis,PLS-DA),探究样品间挥发性成分的差异性。结果表明,通过GC-IMS检测到78个峰,鉴定出59种化合物。通过GC-MS鉴定出94种挥发性化合物,主要挥发性成分是硫化物、烯烃类和醛类。经过干燥后总挥发性化合物的含量显著降低。通过ROAV法确定了(E,Z)-二-1-丙烯基二硫化物、2-巯基-3,4-二甲基-2,3-二氢噻吩、正己醛、2-己烯醛、丁香酚等为香椿样品中关键香气化合物。PCA和PLS-DA结果表明,不同干燥方式的样品与新鲜样品有明显的分离,彼此之间也有明显的区别。鲜样和真空冷冻干燥样品为一组,其他3个干燥香椿样品为一组。根据变量投影重要性(variable importance in projection,VIP)得分共筛选出10种(VIP>1)标志挥发性化合物。干燥方式对香椿风味特性影响显著,真空冷冻干燥组与鲜样最为接近,考虑实际应用热泵干燥为香椿最适宜的脱水方式。本研究为热加工过程中风味品质控制提供一定的理论参考。

两地无花果微量元素及总放射性物质分析与质量评估

目的评估新疆阿图什与江苏南通两地无花果产品质量。方法运用电感耦合等离子体质谱仪和总放测量仪,分别对新疆阿图什和江苏南通两地无花果微量元素和总放射性物质进行分析检测。结果新疆阿图什无花果与江苏南通本地无花果微量元素相比,铝、钾、钙、钒、锰、钴、镍、铜、锌、硒、钡等11种微量元素含量明显较高,镁和钼元素略低,铬元素较低。两地无花果的总α放射性物质和总β放射性物质均合格。结论新疆阿图什无花果产品质量优于江苏南通本地的无花果,具有较高的产品开发价值。

改进和优化黑果枸杞及其制品中花青素测定的pH示差法

建立一种基于美国官方分析化学师协会(Association of Official Analytical Chemists,AOAC)方法检测黑果枸杞及其制品中花青素含量的改进pH示差法。考察了黑果枸杞及其制品中花青素的最佳提取和检测条件,通过液相色谱-三重四级杆串联质谱法鉴别出黑果枸杞中花青素的具体化学结构,并计算出混合花青素的平均摩尔质量。通过分光光度法测得混合花青素的平均摩尔消光系数,对改进后的pH示差法进行方法学验证和花青素的含量测定。结果显示,最佳提取和检测条件如下:黑果枸杞花青素提取溶剂为盐酸-80%(体积分数)乙醇(3∶97,体积比),料液比为1∶100(g∶mL),提取温度为50℃,提取时间为30 min,缓冲溶液稀释5倍后静置平衡20 min。液相色谱-三重四级杆串联质谱法鉴别黑果枸杞中主要以矮牵牛素类花青素为主(占97.96%),黑果枸杞特有的混合花青素平均摩尔质量为912.7 g/mol,平均摩尔消光系数为29591 L/(mol·cm)。pH示差法改进后能够满足方法学验证要求,固体样品和液体样品最低检出限分别为28.2 mg/100 g、0.282 mg/100 mL。方法改进后花青素提取增长率均大于20%,静置平衡20 min后单次检测结果精密度小于0.3%。以矮牵牛素类花青素代替矢车菊素-3-O-葡萄糖苷计算花青素含量平均提高了2.41倍,能真实地反映黑果枸杞及其制品中花青素的含量。

氙同位素丰度参考气制备方法研究

氙同位素丰度比高精度质谱分析技术强烈依赖于氙同位素丰度参考气,参考气的准确制备是关键技术。研究分析了高纯^(128)Xe同位素气体原料中杂质同位素的丰度,采用重量法制备了丰度为80%、91%和92%的^(128)Xe同位素丰度参考气,评定了参考气制备过程引入的不确定度,并采用稀有气体同位素质谱仪对制备的参考气进行验证。结果表明,^(128)Xe同位素丰度参考气制备过程引入的扩展不确定度为0.7%(k=2),制备值与验证值的偏差小于0.2%,表明制备的^(128)Xe同位素丰度参考气量值准确可靠,该同位素丰度参考气能够满足实验室分析质量控制的要求。