鸡肝组织中拉沙洛西钠残留的高效液相色谱检测方法

建立了鸡肝组织中拉沙洛西钠残留的高效液相色谱检测方法。甲醇提取鸡肝组织样品中残留的拉沙洛西钠 ,硅胶柱净化 ,以磷酸盐缓冲液 乙腈 甲醇作为流动相 ,反相高效液相色谱-荧光检测法检测。方法平均回收率为 82 .1 % ,平均变异系数为 7.75 % ,方法的检测限为 0 .0 2mg/kg。

淀粉类油炸食品中丙烯酰胺高效液相色谱检测方法研究

采用HPLC法测定淀粉类油炸食品中丙烯酰胺的含量,样品经水提取后过固相萃取小柱净化,所得净化液选用HPLC-UV外标法检测。本方法丙烯酰胺的检出限为50μg/L,回收率大于92%。

卷烟包装材料中高关注物质色谱检测方法的应用分析

本文通过论述卷烟材料的现状,并就高关注物质色谱检测方法测定卷烟包装材料的应用展开分析,分别从离子色谱法测定烟用纸张中的胆碱、高效液相色谱法测定烟用水基胶中的异噻唑啉酮、正相-高效液相色谱法测定烟用水基胶中壬基酚聚氧乙烯醚三个方面进行研究,旨在最大化消除卷烟包装材料中的有害物质。

食品常用合成色素高效液相色谱检测方法的改进

合成色素在食品当中得到的应用十分广泛,可以改善商品外观并吸引消费者购买,但是合成色素本身没有任何营养。而研究证实合成色素对人体有不同程度的毒性,必须严格控制使用品种、范围和数量,限制每日允许摄入量(ADI),GB 2760许可的有机合成色素基本上都是JECFA规定了ADI值的准许在食品中使用的合成色素,目前需要按照GB 2760的检测方法优化多种合成色素的检测方法。

猪食用组织中喹喔啉-2-羧酸的高效液相色谱检测方法

为了监测猪食用组织中卡巴氧 (carbadox)的残留 ,建立了检测猪肝脏、肾脏、肌肉等组织中卡巴氧的标示残留物喹喔啉 - 2 -羧酸 (Quinoxaline- 2 - carboxylic acid,QCA)的高效液相色谱法。组织样品经碱水解 ,液 -液分配提取 ,用离子交换色谱柱净化 ,洗脱液作浓缩后用甲醇溶解进行测定。色谱柱为 ODS C1 8柱 ;流动相为甲醇 -水 (体积比 4 0∶ 6 0 ) ,每 1L中加入 8m L冰乙酸 ,流速为 1 .0 m L / min;定量分析用紫外检测器 ,波长 32 0 nm,确证性分析用二极管阵列检测器 ,波长 2 5 0～ 5 0 0 nm。喹喔啉 - 2 -羧酸工作液质量浓度在 0 .0 3～ 0 .96 mg/ L 范围内 ,药物峰面积与浓度呈良好的线性关系 ,相关系数 r=0 .9999。组织中添加药物的质量分数为 0 .0 1 5、0 .0 3、0 .0 6μg/ g时 ,肝脏样品回收率分别为 (73.5 5±9.4 6 ) %、(80 .33± 1 4 .95 ) %、(75 .84± 7.4 2 ) % ;肾脏样品分别为 (70 .89± 1 0 .33) %、(74 .89± 7.1 9) %、(83.33±1 0 .6 8) % ;肌肉样品分别为 (6 9.4 9± 7.2 6 ) %、(6 6 .4 4± 5 .0 9) %、(6 2 .1 1± 6 .0 8) %。本方法条件下 ,3种组织中药物最低检出质量分数均为 0 .0 1 5 μg/ g,回收率测定的日内及日间相对偏差 (RSD)分别 <1 8%和 <2 0 %。当组织中药物质量分数达

高效液相色谱-二极管阵列检测方法结合交替三线性分解算法快速定量测定中药黄芩中的黄芩素和汉黄芩素

利用高效液相色谱-二极管阵列检测(HPLC-DAD)方法结合化学计量学基于交替三线性分解算法的二阶校正方法,在未知基体干扰共存下,同时测定了中药黄芩中的黄芩素和汉黄芩素的含量。当体系组分数选取为3时,测得黄芩素和汉黄芩素的平均回收率分别为104.6±4.3%和100.7±7.4%。该方法不仅能同时给出2种物质的相对色谱图和相对光谱图,还能同时测定未知干扰存在下的2种物质的浓度。

食品中合成色素和违禁染料色谱检测的分析研究

在食品检测中,对合成色素和违禁染料的色谱检测方法众多,本文阐述了标准中常用的色谱检测方法,分析了不同标准检测方法中关于样品前处理和分析检测的常见问题,同时比较了不同色谱检测方法的优缺点,探讨了不同色谱检测方法的适用性,并且对食品中合成色素和违禁染料的标准检测方法进行了总结与展望,为未来同类检测研究提供参考。

藏药抱茎獐牙菜HPLC指纹图谱研究

采用反相高效液相色谱-二极管阵列的检测方法,对不同产地的10批野生和栽培抱茎獐牙菜药材的水溶性成分进行了分析,建立了抱茎獐牙菜药材的指纹图谱.色谱柱为VP-ODSC18柱 5μm,150mm×4.6mm ,流动相为甲醇-0.02%的磷酸水溶液,检测波长254nm.用文中的最佳条件可较全面地反映抱茎獐牙菜的主要成分,为藏药抱茎獐牙菜的质量控制提供了科学依据.

藏药花锚指纹图谱研究

采用反相高效液相色谱-二极管阵列的检测方法,对不同产地的10批野生花锚药材的水溶性成分进行了分析,建立了花锚药材的指纹图谱,并对栽培花锚进行了指纹图谱的特征比较.结果证明,栽培花锚中的主要化学成分及数量符合花锚药材的指纹特征,可以代替野生花锚药材入药.

超高效液相色谱-串联质谱法-非衍生化-QuEchERS快速测定奶酪中8种生物胺

目的:建立奶酪中组胺、腐胺、酪胺、尸胺、色胺、β-苯乙胺、精胺和亚精胺的超高效液相色谱-串联质谱检测方法。方法:样品经水提取后,经ODS-H C_(18)色谱柱分离,0.1%甲酸-水、0.1%甲酸-乙腈溶液作为流动相体系梯度洗脱,ESI源电喷雾正离子扫描,多反应监测模式下获得质谱数据,外标法定量。结果:15 min内8种生物胺分离良好,10~2000 ng·mL^(-1)线性良好,相关系数R均≥0.995;检出限为0.05 mg·kg^(-1);定量限为0.15 mg·kg^(-1);奶酪样品中生物胺的回收率为76%~106%,相对标准偏差<10%。结论:该方法操作便捷、快速高效、测定结果可靠,适用于实验室批量样品的检测。

三颗针初提物中盐酸小檗碱含量检测方法研究

采用液相色谱检测方法对三颗针初提物的主要成分盐酸小檗碱进行含量测定,探讨比较单点校正法和外标法两种定量方式.研究表明,两种定量方式与药典规定的滴定法测定盐酸小檗碱含量结果无明显差异,精密度、准确度、回收率均能满足常量检测方法的要求.两种液相分析方法的平均相对标准偏差(RSD)不超过5%,回收率范围集中在70.2%~92.4%之间.考虑到整个实验过程的高效性,在三颗针初提物样品测定盐酸小檗碱成分含量过程中,已知样品大概含量时,可采用单点校正法定量;但不确定样品含量时,推荐使用外标法定量.

Identification of serum proteins discriminating colorectal cancer patients and healthy controls using surface-enhanced laser desorption ionisation-time of flight mass spectrometry

AIM： To detect the new serum biomarkers for colorectal cancer （CRC） by serum protein profiling with surfaceenhanced laser desorption ionisation - time of flight mass spectrometry （SELDI-TOF MS）. METHODS： Two independent serum sample sets were analysed separately with the ProteinChip technology （set A： 40 CRC ＋ 49 healthy controls; set B： 37 CRC ＋ 31 healthy controls）, using chips with a weak cation exchange moiety and buffer pH 5. Discriminative power of differentially expressed proteins was assessed with a classification tree algorithm. Sensitivities and specificities of the generated classification trees were obtained by blindly applying data from set A to the generated trees from set B and vice versa. CRC serum protein profiles were also compared with those from breast, ovarian, prostate, and non-small cell lung cancer. RESULTS： Mass-to-charge ratios （m/z） 3.1×10^3, 3.3× 10^3, 4.5×10^3, 6.6×10^3 and 28×10^3 were used as classitiers in the best-performing classification trees. Tree sensitivities and specificities were between 65% and 90%.Host of these discriminative m/z values were also different in the other tumour types investigated. M/z 3.3× 10^3, main classifier in most trees, was a doubly charged form of the 6.6× 10^3-Da protein. The latter was identified as apolipoprotein C-I. M/z 3.1×10^3 was identified as an N-terminal fragment of albumin, and m/z 28× 10^3 as apolipoprotein A-I. CONCLUSION： SELDI-TOF MS followed by classification tree pattern analysis is a suitable technique for finding new serum markers for CRC. Biomarkers can be identified and reproducibly detected in independent sample sets with high sensitivities and specificities. Although not specific for CRC, these biomarkers have a potential role in disease and treatment monitoring.

Analysis of volatile chemical components of Radix Paeoniae Rubra by gas chromatography-mass spectrometry and chemometric resolution

The volatile chemical components of Radix Paeoniae Rubra (RPR) were analyzed by gas chromatography-mass spectrometry with the method of heuristic evolving latent projections and overall volume integration. The results show that 38 volatile chemical components of RPR are determined, accounting for 95.21% of total contents of volatile chemical components of RPR. The main volatile chemical components of RPR are (Z, Z)-9,12-octadecadienoic acid, n-hexadecanoic acid, 2-hydroxy- benzaldehyde, 1-(2-hydroxy-4-methoxyphenyl)-ethanone, 6,6-dimethyl-bicyclo[3.1.1] heptane-2-methanol, 4,7-dimethyl-benzofuran, 4-(1-methylethenyl)-1-cyclohexene-1-carboxaldehyde, and cyclohexadecane.

Comparison Between MIR and NIR Spectroscopic Techniques for the Determination of Fat and Protein Contents in Milk

To compare mid-infrared(MIR)and near-infrared(NIR)spectroscopies for the determination of the fat and protein contents in milk,the same sample sets with varying concentrations of fat and protein were measured in the MIR range of 3 200-700 cm-1 and NIR range of 9 000-4 000 cm-1.The spectral features in the two regions were analyzed.The MIR spectra of milk were characteristic due to the MIR inherent molecular specificity,whereas the NIR spectra were relatively characterless due to the NIR low selectivity.Partial least squares(PLS)regression models for fat and protein were developed by using both MIR and NIR spectra.MIR data with no pretreatment gave better results than NIR data.The square correlation coefficient(R2)and the root mean square error of prediction(RMSEP)were 0.98 and 0.10 g/dL for fat and 0.97 and 0.11 g/dL for protein.With NIR techniques,satisfactory results were not obtained with raw data.However,NIR data after pretreatment gave similarly good results to the ones using MIR method.This paper indicates that either of the MIR and NIR spectral methods is reliable for the determination of the fat and protein contents.

Quantitative Surface Chirality Detection with Sum Frequency Generation Vibrational Spectroscopy： Twin Polarization Angle Approach

Here we report a novel twin polarization angle （TPA） approach in the quantitative chirality detection with the surface sum-frequency generation vibrational spectroscopy （SFG-VS）. Generally, the achiral contribution dominates the surface SFG-VS signal, and the pure chiral signal is usually two or three orders of magnitude smaller. Therefore, it has been difficult to make quantitative detection and analysis of the chiral contributions to the surface SFG- VS signal. In the TPA method, by varying together the polarization angles of the incoming visible light and the sum frequency signal at fixed s or p polarization of the incoming infrared beam, the polarization dependent SFG signal can give not only direct signature of the chiral contribution in the total SFG-VS signal, but also the accurate measurement of the chiral and achiral components in the surface SFG signal. The general description of the TPA method is presented and the experiment test of the TPA approach is also presented for the SFG-VS from the S- and R-limonene chiral liquid surfaces. The most accurate degree of chiral excess values thus obtained for the 2878 cm^-1 spectral peak of the S- and R-limonene liquid surfaces are （23.7±0.4）% and （-25.4±1.3）%, respectively.

Automatic segmentation of Colon Cancer Cells Based on Active Contour Method： A New Approach

Automatic interpretation of the images of colon cell biopsies requires automatic segmentation of these cells in the image obtained. The active contour method for image segmentation is a well known method for automatic detection of the cell contour. However, the application of this method on colon cell images was not effective. In this paper, the authors have proposed a new technique to reduce the analysis time needed to detect cells in a given image. This technique is based on the active contour method but now using a progressive division of the dimensions of the image to achieve convergence. The model proposed succeeded in detecting cells whose boundaries are not necessarily defined by a gradient. The initial curve can be anywhere in the image, and interior contours can be automatically detected. The developed algorithm was successfully applied on textured multispectral images of three types of cells, including benign hyperplasia （BH）, intraepithelial neoplasia （IN）, and carcinoma （Ca） cells.

Highly Effective Detection of Amitraz in Honey by Using Surface-Enhanced Raman Scattering Spectroscopy Coupled with Chemometric Methods

As an effective and universal acaricide, amitraz is widely used on beehives against varroasis caused by the mite Varroa jacobsoni. Its residues in honey pose a great danger to human health. In this study, a sensitive, rapid, and environmentally friendly surface-enhanced Raman spectroscopy method (SERS) was developed for the determination of trace amount of amitraz in honey with the use of silver nanorod (AgNR) array substrate. The AgNR array substrate fabricated by an oblique angle deposition technique exhibited an excellent SERS activity with an enhancement factor of -10^7. Density function theory was employed to assign the characteristic peak of amitraz. The detection of amitraz was further explored and amitraz in honey at concentrations as low as 0.08 mg/kg can be identified. Specifically, partial least square regression analysis was employed to correlate the SERS spectra in full-wavelength with Camitraz to afford a multiple-quantitative amitraz predicting model. Preliminary results show that the predicted concentrations of amitraz in honey samples are in good agreement with their real concentrations. Compared with the conventional univariate quantitative model based on single peak’s intensity, the proposed multiple-quantitative predicting model integrates all the characteristic peaks of amitraz, thus offering an improved detecting accuracy and anti-interference ability.

小鼠脑组织在氦-氖激光作用下多巴胺的变化

目的 探讨氦－ 氖激光对小鼠脑组织多巴胺有无影响；方法 在麻醉状态下，切开小鼠头部皮肤，暴露颅骨及脑组织，用氦－ 氖激光仪垂直照射小鼠额叶皮质，采用高效液相色谱－ 电化学检测方法测定不同剂量氦－ 氖激光照射后小鼠脑组织多巴胺含量的变化；结果 激光照射各组可明显增加小鼠脑组织ＤＡ 含量，以剂量为５５ ．１Ｊ／ｃｍ２ 和２７ ．６Ｊ／ｃｍ２ 组最明显， 差异有高度统计学意义；结论 氦－ 氖激光脑局部照射可增加小鼠脑组织ＤＡ 含量，且与激光剂量有关。

HPLC-CAD法测定芪蛭通络胶囊中苷类成分的含量

目的 建立高效液相色谱-电喷雾检测器方法(HPLC-CAD)同时测定芪蛭通络胶囊中人参皂苷Rb_(1)和黄芪甲苷的含量。方法 采用色谱柱为Waters XSclectHss T3-C_(18)(4.6 mm×250 mm,5μm),水(A)-乙腈(B)为流动相,梯度洗脱(0 min,15%B;0~10 min,15%~25%B;10~15 min,25%B~31%B;20~50 min,31%B),流速1 mL·min^(-1),柱温25℃,进样量为20μL。电喷雾检测器(CAD)雾化器温度为35℃,功能参数(power function,PF)为1.0。结果 芪蛭通络胶囊中人参皂苷Rb_(1)和黄芪甲苷均具有良好的线性关系(r>0.999 0),定量限(LOQ)分别为0.013和0.015μg,精密度、重复性、24 h稳定性实验的相对标准偏差(RSD)值均小于3.0%,平均加样回收率分别为91.74%和100.09%。结论 本研究建立的HPLC-CAD法可同时对芪蛭通络胶囊中人参皂苷Rb_(1)和黄芪甲苷进行含量测定,为芪蛭通络胶囊的检测分析和质量控制提供了新的方法。