化妆品中双香豆素和环香豆素的高效液相色谱二极管阵列检测器测定

建立了用高效液相色谱(HPLC)/二极管阵列检测器(DAD)测定化妆品中两种香豆素物质--双香豆素和环香豆素的方法.样品用乙腈-氢氧化钠溶液(0.1 mol/L)(体积比9:1)的提取溶液超声提取,高效液相色谱DAD扫描检测,并在306 nm波长进行分析.用保留时间结合二种香豆素的紫外光谱定性,外标法定量,并且采用液质联用(LC-MS/MS)确证.双香豆素的回收率为96%～105%,精密度RSD为0.51%～2.08%,定量下限为1 ng;环香豆素的回收率为88%～104%,精密度RSD为0.51%～3.36%,定量下限为1 ng.     

高效液相色谱法测定血红蛋白氧载体中残留的戊二醛

建立了一种测定血红蛋白氧载体中戊二醛残余含量的高效液相色谱方法.用10 kDa超滤膜通过离心3000 r/min×20 min将游离戊二醛从待测样品中分离;在pH 1.0时,在含有70%乙腈的体系中用2,4-二硝基苯肼在30 min内将戊二醛衍生成2,4-二硝基苯腙(n(2,4-二硝基苯肼): n(戊二醛)=60: 1),以70%乙腈为流动相,避免了衍生产物生成沉淀.用高效液相色谱法分离测定衍生物,可在20 min内完成分离,同时对衍生步骤进行了优化.本方法具有较高的灵敏度和良好的线性关系,检出限为1.0 ng,在0.1～10 mg/L范围内其线性相关系数为0.9999,重复测定6次的相对标准偏差小于3.0%,回收率为95.26%.     

高效液相色谱法测定硝基涂料中的增塑剂邻苯二甲酸酯类

建立了用高效液相色谱法测定硝基涂料中的邻苯二甲酸酯类化合物的方法。样品待挥发性有机物挥发后,用乙醇提取其中的邻苯二甲酸酯类,直接用HPLC分析,外标法定量。该方法的精密度为2 05%～4 93%,回收率为79 5%～106 0%,检出限为DMP0 14ng,DEP0 22ng,DBP0.61ng。     

高效液相色谱法对唇膏中9种限用着色剂的同时测定

建立了用高效液相色谱/二极管阵列检测器(HPLC/DAD)同时测定唇膏中9种限用着色剂(溶剂绿7、食品黄3、食品红17、酸性黄1、酸性红33、食品红4、食品红1、橙黄Ⅰ和酸性橙7)的检测方法.采用C18反相色谱柱,以乙腈-磷酸二氢钾缓冲溶液(pH 6.0)为流动相进行梯度洗脱,用DAD检测器扫描检测.以保留时间结合待测物的紫外吸收光谱进行定性分析,采用外标法进行定量分析,定量检测波长240 nm.所建方法可在15 min内对9种目标物同时进行检测,且各化合物均达到基线分离.实验结果表明,在0.05 ～100 mg/L范围内,9种着色剂的质量浓度与相应的峰面积比值呈良好的线性关系.方法的平均回收率(n=9)为85% ～100%,相对标准偏差(RSD)为3.68% ～8.20%,9种目标物的检出限为0.01 ～0.1 mg/L.     

固相萃取-超高效液相色谱串联质谱法测定食品中碱性橙、碱性嫩黄O

建立了固相萃取-超高效液相色谱串联质谱法同时检测食品中碱性橙、碱性嫩黄O的方法,样品提取液采用C18固相萃取柱净化,用超高效液相色谱-串联质谱法在3 min内完成分离检测.碱性橙、碱性嫩黄O方法检出限(S/N=3)分别为0.34、1.28μg/kg;定量下限(S/N=10)分别为1.13、4.27μg/kg.回收率为80.1%～95.3%.方法分析时间短、灵敏度高且准确可靠,能满足食品中低含量碱性橙、碱性嫩黄O的同时定性定量分析要求.     

高效液相色谱-荧光检测法测定环境水中的苯胺和苯酚

建立了用高效液相色谱荧光检测法同时测定环境水中苯胺和苯酚的分析方法。色谱柱为EclipseXDB C8(4.6mmi.d.×150mm,5μm),流动相为甲醇 磷酸盐缓冲液(0.1mol/L磷酸二氢钾 0 1mol/L磷酸氢二钠,pH6.87)V(甲醇)∶V(磷酸盐缓冲液)=50∶50,流速1 0mL/min,柱温25℃,检测波长0minλex/λem=230/340nm(测定苯胺),3.5minλex/λem=215/300nm(测定苯酚)。测定苯胺的线性范围0.2～120ng,r=0.9999,检出限0.01ng;测定苯酚的线性范围0.4～500ng,r=0.9998,检出限0.02ng,回收率98.1%～101.2%。该方法已用于对环境水中苯胺和苯酚的测定。     

塑料玩具中酚类环境雌激素在模拟汗液和唾液中溶出行为研究

建立了快速溶剂萃取-超高效液相色谱法同时测定塑料玩具中5种环境雌激素(EES)的分析方法。将塑料玩具样品剪碎后,用二氯甲烷作溶剂经快速溶剂萃取、浓缩、过滤,用超高效液相色谱ACQUITY UPLC-BEHC18柱(50 mm×2.1 mm,1.7μm)分离,以乙腈-水为流动相,梯度洗脱,流速0.4 mL/min;检测波长200 nm,外标法定量。该方法回收率为93.7%～98.2%,测定结果的相对标准偏差为0.4%～2.1%(n=6),检出限为0.11～0.42ng/mL。此方法可作为测定塑料玩具中酚类环境雌激素的分析方法。     

基质固相分散-HPLC双柱测定辣椒油中苏丹红

建立辣椒油中苏丹红Ⅰ～Ⅳ残留分析的高效液相色谱法.样品通过基质固相分散(MSPD)快速萃取净化,Novapak C18(3.9×250 mm,5 μm)进行分离,用双波长紫外/可见检测器进行检测,波长为478和520 nm,对于阳性样品通过双柱进行确认.回收率在80.8%～91.9%,相对标准偏差为2.1%～6.0%,最低检测限为0.5 ng.     

自动固相萃取/高效液相色谱-质谱/质谱检测动物源性食品中残留二苯乙烯类激素的方法研究

应用自动固相萃取仪(ASPE)/高效液相色谱-质谱/质谱仪(HPLC-MS/MS)同时分析动物源性食品中残留二苯乙烯类激素——己烯雌酚(DES)、己烷雌酚(HEX)、双烯雌酚(DEN)。样品净化采用装配硅胶固相萃取柱的ASPE,液相色谱分离用C8柱,大气压化学模式电离,多反应离子监测方式检测,DES-d8同位素标记物做内标定量。方法对DES、DEN的检出限为0.05ng.g-1,在0.5~10ng.g-1范围内回收率为84%~108%;对HEX的检出限为0.025ng.g-1,在0.25~5ng.g-1范围内回收率为59%~87%。     

高效液相色谱检测反应香精中的2-氨基-N-甲基-5-苯基咪唑并吡啶(PhIP)方法研究

建立了用高效液相色谱快速检测反应香精中2-氨基-N-甲基-5-苯基咪唑并吡啶的方法. 反应香精中的2-氨基-N-甲基-5-苯基咪唑并吡啶用二甲基甲酰胺直接超声振荡提取; 高效液相色谱的色谱柱为Eclipse XDB-C18 (250 mm×4.6 mm, 5 μm); 流动相为V(二甲基甲酰胺)∶V(甲醇)∶V(水)=8∶50∶42; 流速为0.5 mL/min; 光电二极管阵列检测器检测波长为UV-327 nm. 10种反应香精中均未检出该种物质, 回收率为78.9%～85.9%, 检出限为19.2 ng/mL.     

薄层色谱扫描法测定塑料食品袋中酞酸酯的含量

建立了采用薄层色谱扫描测定塑料食品袋中4种酞酸酯(酞酸二甲酯(DMP)、酞酸二乙酯(DEP)、酞酸二丁酯(DBP)和酞酸二(2-乙基己基)酯(DEHP))的方法。经粉碎的样品先用乙醇浸泡24 h,然后超声提取,经0.45 μm滤膜过滤。点样在以丙酮处理过的硅胶G板上,以乙酸乙酯-无水乙醚-异辛烷(体积比为1∶4∶15)为展开剂展开,以双波长反射吸收飞点扫描测定(λS=275 nm,λR=340 nm),外标法定量。该法的线性关系较好，DMP、DEP、DBP和DEHP的检出限分别为2.1,2.4,3.4和4.0 ng,混合标准品在同一薄层板上的峰面积的相对标准偏差（RSD）为2.8%～3.5%，4种酞酸酯的样品加标回收率为78.58%～111.04%。该方法样品用量少,前处理简单,分离效果好,可用于塑料袋中4种酞酸酯的同时测定。经与气相色谱法的分析结果比较，两种方法对实际样品的分析结果接近。     

Leakage of gaseous 125I from a Na125I solution through a plastic film

Leakage of gaseous 125I from the various kinds of plastic film bags packing Na125I solution was determined. The polyethylene bag was permeable to the gaseous 125I and active charcoal could not prevent the leakage. The laminated plastic bags composed of polyethylene terephthalate and polyethylene was slightly permeable, and the leakage decreased either in the presence of active charcoal or with the use of doubly packed bags. Leakage of 125I from the various kinds of container for the Na125I solution was also determined.     

Butyltin compounds in vinegar collected in Beijing: Species distribution and source investigation

Forty-eight vinegar samples including white vinegar,rice vinegar and mature vinegar were collected from several markets in Beijing.Butyltin compounds were determined by headspace solid-phase microextraction coupled with gas chromatography and flame photometric detector after in situ ethylation with sodium tetraethylborate.Butyltin species were detected in sixteen vinegar samples and ranged from 0.012 to 14.10 μg Sn L 1.The detection rate of white vinegar is higher than that of rice vinegar and mature vinegar.Vinegar samples with relatively high butyltin concentration(>1.5 μg Sn L 1) were those stored in plastic bags,indicating that the plastic bag was one of the possible sources of butyltin contamination.This was further confirmed by the leaching experiments of three selected plastic bags,and monobutyltin was detected in the leaching solvents.According to the estimation,the average daily intake of total butyltin compounds through vinegar consumption is about 0.04 ng Sn/kg b.w.,much lower than the Tolerable Daily Intake(TDI) of 100 ng Sn/kg b.w.set by the European Food Safety Authority(EFSA).     

Quantitation of hyaluronic acid and chondroitin sulphates in rabbit synovial fluid by high-performance liquid chromatography of oligosaccharides enzymatically derived thereof

A high-performance liquid chromatographic (HPLC) method for quantifying unsaturated hexasaccharide and tetrasaccharide from Streptomyces hyaluronidase enzyme digestion products of hyaluronic acid was developed using a gel-permeation column packed with a sulphated polystyrene-divinylbenzene gel. For the oligosaccharides, the separation was accomplished in less than 7 min with a detection limit of 65 ng. An unsaturated non-sulphated disaccharide prepared from hyaluronic acid (delta Di-HA) and an unsaturated sulphated disaccharide (delta Di-4S) were analyzed by a HPLC method using a combination of two different gel-permeation columns. The separation of the disaccharides required less than 17 min at a flow rate of 0.7 ml/min with detection limits of as little as 4 ng for delta Di-HA and 5 ng for delta Di-4S. Both chromatographic methods were used for assay of a major component of hyaluronic acid and trace amounts of chondroitin sulphates in rabbit synovial fluid. The resulting contents of hyaluronic acid were compared to the values of polymeric hyaluronic acid directly measured by a HPLC method using two gel-permeation columns packed with a poly(hydroxyalkyl methacrylate) gel and the amounts of hyaluronic acid converted from uronic acid content determined by a colorimetric method.     

Determination of bradykinin and arg-bradykinin in rat muscle tissue by microdialysis and capillary column-switching liquid chromatography with mass spectrometric detection

Quantification of bradykinin peptides in limited amounts of rat muscle tissue dialysate has been performed using a packed capillary LC-ESI-TOF-MS method. The micro dialysate samples (450 microL) with added internal standard were loaded onto a 1 mm x 5 mm loading column packed with 5 microm Kromasil C18 particles by a carrier solution of 0.1% formic acid in ACN/water (5:95, v/v) at a flow rate of 250 microL/min for online preconcentration of the analytes. Back-flushed elution onto a 150 mm x 0.5 mm Zorbax C18 column packed with 5 microm particles was conducted using a linear solvent ACN/H2O gradient containing 0.1% formic acid. (Tyr8)-bradykinin was used as an internal standard and was added to the dialysis sample prior to injection. Baseline separation of bradykinin, arg-bradykinin and (tyr8)-bradykinin was achieved within 10 min. Positive ESI was performed in the m/z range of 200-1300. The method was validated in the range 0.2-1.0 ng/mL dialysate, yielding correlation coefficients of 0.995 and 0.990 for bradykinin and arg-bradykinin, respectively. The within-assay and between-assay precisions were between 4.3-9.6% and 6.2-10.6%, respectively. Both arg-bradykinin and bradykinin were detected in dialysate from rat muscle tissue, at concentrations of 0.1 and 0.4 ng/mL for bradykinin and arg-bradykinin, respectively, confirming the presence of arg-bradykinin in rat muscles.     

Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction,aqueous acetylation and microextraction by packed sorbent

We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi–GC/MS. A washed hair sample (1–5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 μL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 μL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20–50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20–30 times use. The carry over was estimated to be about 1–2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods.     

气相色谱法测定塑料食品包装袋中甲苯残留

 提出一种食品塑料包装袋中残留甲苯的气相色谱分析方法。     

Panus tigrinus strains used in delignification of sugarcane bagasse prior to kraft pulping

Three strains of the white-rot fungus Panus tigrinus (FTPT-4741, FTPT-4742, and FTPT-4745) were cultivated on sugarcane bagasse prior to kraft pulping. Pulp yields, kappa number, and viscosity of all pulps were determined and Fourier transform infrared (FTIR) spectra from the samples were recorded. The growth of P. tigrinus strains in plastic bags increased the manganese peroxide and xylanase activities. Lignin peroxidase was not detected in the three systems (shaken and nonshaken flasks and plastic bags). FTIR spectra were reduced to their principal components, and a clear separation between FTPT-4742 and the control was observed. Strain FTPT-4745 decayed lignin more selectively in the three systems utilized. Yields of kraft pulping were low, ranging from 20 to 45% for the plastic bag samples and from 12 to 38% for the flask samples. Kappa numbers were 1–18 and viscosity ranged from 2.3 to 6.8 cP.     

Microextraction by packed sorbent of N-nitrosamines from Losartan tablets using a high-throughput robot platform followed by liquid chromatography-tandem mass spectrometry

The development of a fast, cost-effective, and efficient microextraction by packed sorbent setup was achieved by combining affordable laboratory-repackable devices of microextraction with a high-throughput cartesian robot. This setup was evaluated for the development of an analytical method to determine N-nitrosamines in losartan tablets. N-nitrosamines pose a significant concern in the pharmaceutical market due to their carcinogenic risk, necessitating their control and quantification in pharmaceutical products. The parameters influencing the performance of this sample preparation for N-nitrosamines were investigated through both univariate and multivariate experiments. Microextractions were performed using just 5.0 mg of carboxylic acid-modified polystyrene divinylbenzene copolymer as the extraction phase. Under the optimized conditions, the automated setup enabled the simultaneous treatment of six samples in less than 20 min, providing reliable analytical confidence for the proposed application. The analytical performance of the automated high-throughput microextraction by the packed sorbent method was evaluated using a matrix-matching calibration. Quantification was performed using ultra-high-performance liquid chromatography-tandem mass spectrometry with chemical ionization at atmospheric pressure. The method exhibited limits of detection as low as 50 ng/g, good linearity, and satisfactory intra-day (1.38–18.76) and inter-day (2.66–20.08) precision. Additionally, the method showed accuracy ranging from 80% to 136% for these impurities in pharmaceutical formulations.