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CFAPA401米粉中钾钙钠镁铁锌磷能力验证

http://simg.instrument.com.cn/bbs/images/default/emyc1007.gif支持分坛团队和化学药分析版。我公司产品注射用帕米膦酸二钠执行标准为《中国药典》2010年版二部。含量测定项下的内容为：“【含量测定】照离子色谱法（附录 V J）测定色谱条件与系统适用性试验用阴离子交换色谱柱；以3mmol/L草酸溶液为流动相，流速为每分钟1.2ml；检测器为电导检测器。理论板数按帕米瞵酸二钠峰计算不低于2000。”我们在检测中发现，含量测定色谱柱的理论塔板数下降较快。经研究，将流动相由“3mmol/L草酸溶液”改变为“**溶液”，可使柱效明显稳定。方法学验证结果显示，变更后的方法准确、可靠。可用于我公司产品注射用帕米膦酸二钠含量测定。1仪器与试药1.1仪器岛津LC-20A高效液相色谱仪，配CDD-10A VP电导检测器。所用仪器和量具均经校准或检定。1.2试药对照品帕米膦酸二钠（经160℃干燥至恒重，按干燥品计含量100.2%，按100%计。）。辅料、水为超纯水。2方法与结果2.1色谱条件色谱柱Dionex IonPac AS22阴离子交换色谱柱（4 mm ×250 mm），配保护柱（4 mm ×50 mm）；流动相**溶液；检测器为电导检测器；柱温35℃；流速1.2ml/min。进样量为20μl。理论塔板数按帕米膦酸二钠峰计算应不低于2000。2.2溶液的制备2.2.1空白辅料储备液：取辅料适量，按处方配成溶液备用。2.2.2空白辅料溶液：取空白辅料储备液5ml置于50ml容量瓶中，加水定容至刻度。2.2.3对照品溶液：精密称取帕米膦酸二钠对照品约30mg，置于50ml容量瓶中，用水溶解并定容。2.2.4供试品溶液：精密称取帕米膦酸二钠对照品适量（根据不同验证项目，称取不同量），置于50ml容量瓶中，加水溶解后，加入5ml空白辅料储备液并用水定容。2.3专属性试验空白溶剂：水。取空白溶剂、空白辅料溶液、对照品溶液、供试品溶液，照2.1色谱条件，依法测定，记录色谱图。（附图略）结果显示，对照品溶液和供试品溶液的色谱图中帕米膦酸二钠峰与其他峰之间分离度良好，分离度大于1.5；空白溶剂及空白辅料溶液色谱图中在帕米膦酸二钠峰处无干扰峰。本方法有良好的专属性。2.4 线性关系及范围精密称取帕米膦酸二钠对照品14.58、24.28、30.58、36.13、45.80 mg，分别置50ml量瓶中，用水适量溶解后，加入5ml空白辅料储备液并用水定容，摇匀，制成每1ml中含帕米膦酸二钠0.2916、0.4856、0.6116、[/fon

http://simg.instrument.com.cn/bbs/images/default/emyc1007.gif这是很久以前做的一个方法，拿来参加原创大赛，支持液相色谱版。由于涉及公司产品，文中部分信息隐去，请见谅。--------------------------------------------------------------------------------------------------HPLC测定注射用帕米膦酸二钠中的亚磷酸含量 注射用帕米膦酸二钠的原料帕米膦酸二钠结构稳定，对光、热等均不敏感，正常的储存条件下不易产生降解产物。亚磷酸作为帕米膦酸二钠的合成原料，属于制剂中的有关物质。我们参考相关资料，对注射用帕米膦酸二钠中的亚磷酸含量测定进行了研究。测定法：“取本品，加水制成每1ml中含帕米膦酸二钠10mg的溶液，摇匀，滤过，作为供试品溶液；另取亚磷酸适量，精密称定，加水制成每1ml中约含0.05mg的溶液，作为对照品溶液。照高效液相色谱法测定，用阴离子色谱柱；以**溶液为流动相，示差检测器检测；柱温为35℃，流速为1.0ml/min。取对照品溶液和供试品溶液各50μl注入液相色谱仪，供试品溶液的色谱图中如出现与对照品溶液相应的杂质峰，其峰面积不得大于对照品溶液主峰面积（0.5％）”仪器与试药：LC-10A液相色谱仪配示差检测器，亚磷酸对照品购自SIGMA。线性：取亚磷酸对照品0.1020g，加水溶解并稀释至100ml，分别精密量取1，2，3，4，5ml，置100ml量瓶中，加水至刻度，摇匀，制备成约含亚磷酸10，20，30，40，50mg/L的标准曲线序列，依法测定：浓度mg/L峰面积10.20799120.401559730.60[font=Times

CFAPA401婴幼儿米粉中钾钙钠镁铁锌磷QQ群：680336409

各位，有没有一种色谱柱即可以测PAHs,邻苯15P，又可以测多溴联苯醚；且分离效果好？我现在用的GC-MS是岛津QP2010plus。

我手上有1、GB植物性食品中甲胺磷的检测方法；2、动物性食品中甲胺磷的检测方法；3、CDPA-MRSM（美国加州食品农业部）；4、FDA；5、日本（肯定列表制度）。 我想大家来讨论玉米甲胺磷的提取、净化、浓缩方法，我想玉米毕竟成分不算太复杂（玉米主要是含碳水化合物）。 举个例子：提取方法有乙腈法—CDFA（US）；丙酮法—FDA（US）；乙酸乙酯法—欧盟法；混合溶剂法（乙腈-丙酮-甲醇） — FDA（US）等，大家来讨论出最好最有效的方法。

【序号】： 1【作者】： [url=http://search.cnki.com.cn/Search.aspx?q=author:%E4%B8%A5%E5%85%A8%E9%B8%BF][color=#0365bf]严全鸿[/color][/url] [url=http://search.cnki.com.cn/Search.aspx?q=author:%E9%92%9F%E6%96%B0%E6%9E%97][color=#0365bf]钟新林[/color][/url] 【题名】： [url=https://insevent.instrument.com.cn/t/3p][color=#3333ff]离子色谱[/color][/url]法测定帕米膦酸二钠注射液的含量【期刊】： 中国卫生检验杂志【年、卷、期、起止页码】： [size=2]2009, 19(01) :48-49,66[/size]【全文链接】：[url=http://www.cnki.com.cn/Article/CJFDTotal-ZWJZ200901019.htm][color=#0365bf]http://www.cnki.com.cn/Article/CJFDTotal-ZWJZ200901019.htm[/color][/url]

7. Linearity and Detection LimitsThe next few parts of this guide will provide practical information for the operator in the realization and demonstration of the key performance characteristics designed into their ICP by the manufacturer.I have personally had the opportunity to see the advancement of ICP instrumentation over the past 30 years. Current instrumentation and software provided by manufacturers has gone well beyond anything I could have imagined 30 years ago (and it costs less). In 2004 it takes $3.21 to purchase what cost $1.00 in 1975, yet during this time period the price of ICP instrumentation has gone down while the performance characteristics have improved by orders of magnitude. A 憄ersonal experience?example is the detection limit for K by ICP-OES that has gone from 0.4 ppm to 1 ppb where the 0.4 ppm detection limit was measured on an instrument that in 1975 cost 1.5 times the 2000 price of the instrument that measured the 1 ppb detection limit (taking inflation into account, the 2000 price would be one fifth the 1975 price).Although an ICP instrument can be wheeled into a laboratory and begin collecting data the same day, the operator is encouraged to realize and demonstrate the key performance characteristics of linearity, detectability, and spectral integrity and then go on to make decisions based upon the boundaries of these performance characteristics and the limitations of the analytical problem. Defining and being able to realize your instrument抯 performance characteristic is an investment that will save time over the years to come and allow you to make the right choices.Defining ICP Performance Characteristics The following steps are intended as a practical guide for the determination of an ICP抯 performance characteristics:Read the operating manual and familiarize yourself with the software, key instrumental parameters and preferred settings before the instrument is installed. Most instruments are supplied with optimization and wavelength or mass calibration standards that will be used during set-up by the service technician and are intended for use on a regular basis by the operator. Discuss the optimization process with the manufacturer as well as the preferred settings for the key instrumental parameters.The remaining steps assume that the operator fully understands and is able to perform the optimization process that has been defined by the manufacturer as well as the spectral limitations of the instrument.Select the lines to be studied for each element (憀ines?is used in this document to mean either wavelength or mass). Line selection is based upon spectral interference issues, detection limit requirements and working range requirements. Select as many lines as possible within practicality for each element. The greater the number of lines, the greater the flexibility.Prepare single element standards over the anticipated working range for each element. The range of standards depends upon the analytical requirements. The following ranges are suggestions only:• Radial view ICP-OES: 0.0, 1, 10, 100, and 1000 礸/mL• Axial view ICP-OES: 0.0, 0.1, 1, 10, and 100 礸/mL• Quadrupole (R~ 300) mass filtered [url=https://insevent.instrument.com.cn/t/yp][color=#3333ff]ICP-MS[/color][/url]: 0, 1, 10, 100, and 1000 ng/mLThis step is important because these data can be used to determine instrument detection limits (IDL), linear working ranges, and spectral characteristics such as background equivalent concentrations (BEC) and spectral interferences. With most modern (if not all) instruments, the spectra obtained for each element at each concentration can be saved for review later. In addition, the software will calculate the IDL and BEC plus the linear regression of each line will establish the linear working range. All of this is typically done for the operator by the software that comes with the instrument. If at all possible, attempt to:Use single element standards that have the trace metals impurities reported on the certificate of analysis. Most chemical standards manufacturers provide this information with their single element standards. These data are important in identifying direct spectral overlap interferences and in not identifying an impurity as an interference of this type.Store all spectra on computer and collect the spectra for all lines of interest on each and every solution. This means that if you are interested in possibly using up to 6 lines for roughly 72 elements, then each solution spectrum totaling 72 x 6 = ~ 432 lines per solution and ~ 432 x 5 = 2160 spectra for each element need to be stored for future reference. Most [url=https://insevent.instrument.com.cn/t/yp][color=#3333ff]ICP-MS[/color][/url] applications would require far fewer data to be collected due to the reduced number of lines available and/or feasible.Wash blank acid solution through the instrument for several minutes 慴etween elements?and always analyze a blank at the beginning of each element concentration series. Look for the presence of the prior element analyzed to confirm that it has been completely washed out of the introduction system.Having the data available on a desktop computer is convenient and allows the analyst to construct potential spectra by calling up the element and the anticipated concentration for each element in the analytical sample. Having several lines available makes the job of line selection easy as well as the estimation of the line抯 sensitivity and linearity. Constructing these composite spectra from pure single element solutions eliminates confusion as to the identity of the line. The following example is intended to illustrate the process:Examples of Spectra:NOTE: All spectra were obtained using a concentric glass nebulizer with no problems around salting out or plugging.The following example is for an application where a submitter has been obtaining minor levels (0.1 to 1.0 %) of Cr in an alloy containing roughly equal amounts of Fe and Ni. The laboratory where this alloy is analyzed uses a procedure where 0.2 grams of the sample is dissolved in 5 mL of a 1:1 HNO3 / HCl mixture and diluted to 1000 mL with DI water. The analyst is informed that a limit of detection (LOD = 3SD0) of 1 ppm Cr based upon the original sample and the ability to quantify the Cr to within &plmn 10 % relative at the 10 ppm level is an absolute minimum requirement.The submitter then asks the analyst the usual question, 揑 need the results tomorrow ?can you do it??The analyst does a quick calculation and determines that using the most sensitive Cr line and the current procedure, the lowest possible detection limit is 4 ppm and a more realistic estimation would be ~ 4 times the IDL or ~ 16 ppm. The analyst then pulls up the following spectra, instrument detection limits, and linear regression data which were obtained on their radial view instrument about four years ago when installed using pure single element solutions as described above.

中国科技网讯 据美国每日科学网站近日报道，美国科学家研发出一种名为D2PA的人造纳米材料，将这种材料同用来探测疾病的免疫分析方法相结合，能将这种标准的生物学工具的灵敏度提高300万倍。最新突破将大大改进癌症、阿尔茨海默症等疾病的早期探测情况，因为医生能探测到浓度更低的疾病生物标签。研究发表在最新一期《纳米技术》杂志上。 免疫分析方法这一医学测试主要通过模拟免疫系统的行为来探测生物标签（与疾病有关的化学物质）在样本内的分布情况。当生物标签出现在从人体内提取的样本中时，该免疫分析测试会发出闪闪荧光，实验室可以探测到这些荧光的踪迹。荧光越亮，表明生物标签越多。然而，如果生物标签太少，荧光就会非常微弱从而无法被探测到。免疫分析研究的主要目标之一就是改进探测效率。 现在，普林斯顿大学的科学家们借用纳米技术，大大增强了样本中微弱的荧光，将探测灵敏度提高了300万倍。也就是说，与传统方法相比，改进后的免疫分析方法在生物标签少300万倍的情况下，也可以进行很好的探测。 该研究的领导者、普林斯顿大学工程学院的教授史蒂芬·周表示：“最新突破为免疫分析方法和其他探测方法以及疾病的早期探测和诊断、治疗提供了很多新机会；另外，新方法使用起来也非常方便。”该研究由美国国防部高级研究计划局和美国科学基金会资助。 最新研究取得突破的关键在于科学家们研制出的人造纳米材料D2PA。D2PA是一层薄薄的金纳米结构，其周围被直径仅为60纳米的玻璃柱所环绕，这些玻璃柱每隔200纳米放置一个，每个柱子上都覆盖有一层金。每个柱子的周边都散落着更细小的、直径仅为10纳米到15纳米的金点。在以前的研究中，史蒂芬·周已经证明，这个独特的结构能采用非比寻常的方法提升光的聚合和传输能力，尤其是其可以将表面拉曼散射的效率提高10亿倍。而最新研究也证明，该结构能大大增强荧光信号。 免疫分析除了应用于诊断领域之外，还能广泛用于药物研发和其他生物学研究领域。史蒂芬·周表示，荧光在化学和工程学领域都起着重要的作用，可应用于从发光显示器到太阳能捕获设备等之上，D2PA材料在这些领域也能找到“用武之地”。 史蒂芬·周表示，接下来，他打算进行一些测试，比较D2PA增强的免疫分析方法和传统方法在乳腺癌和前列腺癌方面的测定灵敏度。另外，他也在和纽约史丹基达宁癌症研究中心的科学家们携手合作，研发测试同极早期阿尔茨海默症有关的蛋白质。他说：“使用我们的最新方法，能够很早探测出阿尔茨海默症。”（刘霞） 《科技日报》（2012-06-08 二版）

大家对EPA8270D有米有什么不懂得？ 大家的测试方法是不是从其中转过来的啊 你们的方法是仪器厂商给的还是自己做得？如果是你坐得你有事如何做得啊？

【序号】：1【作者】：A. R. A. Palmans, J. A. J. M. Vekemans, E. W. Meijer【题名】：Intramolecular hydrogen bonding in acylated 2,2′-bipyridine-3,3′-diamines【期刊】：Recueil des Travaux Chimiques des Pays-Bas【年、卷、期、起止页码】：Volume 114, Issue 6, pages 277–284, 1995【全文链接】：http://onlinelibrary.wiley.com/doi/10.1002/recl.19951140605/pdfhttp://onlinelibrary.wiley.com/doi/10.1002/recl.19951140605/abstract;jsessionid=0DCA97D1D37C7AC52911DDFD80443438.d03t04

各位版友 有两个问题 因为首次做水质常规，需要大家帮忙解答1、现有的环境监测法规，GB/T 11893-1989测定总磷，HJ 636-2012测定总氮时，是否可以使用民用高压锅?是否一定需要可控温可定时的高温蒸汽灭菌锅?如果使用民用高压锅(通常1.7MPa-1.9MPa)，那么如何实现法规中的120摄氏度30分钟?我们是需要申请CMA和CNAS资质的，所以需要有对应的法规，并且要做方法验证报告。2、我们使用密闭消解法做COD，这种消解仪和消解管也可以用来做总氮、总磷，那么想问如果用比色管法做总氮、总磷是否符合GB/T 11893-1989测定总磷，HJ 636-2012测定总氮的要求?或者有其他对应的法规?理论上如果自己做研究技术都是做的通的，问题是我们要做资质申请，想了解和法规的符合情况，如果不符则需要进行方法比对和验证。

请问有参加FAPAS今年2月27发出的大米粉重金属能力比对吗？我们测铅、镉，第一次参加FAPAS，想和大家交流下

【序号】：1【作者】：Linda M. Thienpont, Jean E. Van Nuwenborg, Hans Reinauer and Dietmar Stöckl【题名】：Validation of candidate reference methods based on ion chromatography for determination of total sodium, potassium, calcium and magnesium in serum through comparison with flame atomic emission and absorption spectrometry【期刊】：Clinical Biochemistry【年、卷、期、起止页码】：Volume 29, Issue 6, December 1996, Pages 501-508【全文链接】：http://www.sciencedirect.com/science/article/pii/S0009912096000902

最近听说安东帕DMA38的密度计使用起来不错。不知使用的大侠们，感觉怎样？分享一下。另外，大概价位在多少？

帕拉米韦注射液已经获批用来治疗H7N9禽流感。不知道这个获批是正常获批，还是因为这次疫情的爆发，非常时刻顶上去的。你们觉得有保证吗？

各位大佬们，求购topas-academic V4.1及以上版本的软件，哪位大佬有多余的软件能够出售。或寻人共同购买官方渠道的topas-academic V6，多人购买价格优惠。

那位大侠有王中林纳米材料手册,谢谢

【序号】：【作者】：Peter P. T. Sah, T. C. Daniels【题名】：Thiosemicarbazide as a reagent for the identification of aldehydes, ketones, and quinones【期刊】：Recueil DES Travaux Chimiques DES Pays-Bas. 【年、卷、期、起止页码】：1950,69(12):1545-1556【全文链接】：http://onlinelibrary.wiley.com/doi/10.1002/recl.19500691211/abstract

不知DCP-AES,MIP-AES,GC-MIP前景如何啊?以后能不能与ICP-AES相抗衡?

【题名】：Near infrared spectroscopy for rapid and in-line detection of particle size distribution variability in lactose during mixing【期刊】：【年、卷、期、起止页码】：【全文链接】：https://doi.org/10.1016/j.ijpharm.2019.06.002

大师王中林发表在Advanced Functional Materials上关于氧化物压电纳米结构的文章，电镜照片堪称艺术品。读后，相信对晶体学，电子显微学基本概念有所帮助。