塑料玩具中7种环境雌激素含量检测

目的 了解塑料玩具类制品中邻苯二甲酸酯类（PAEs）、双酚A（BPA）和壬基酚（NP）的含量。方法 四氢呋喃溶解甲醇沉淀法处理玩具样品，用反相高效液相色谱（RP-HPLC）进行分离测定。结果 所有玩具均检出2种以上的雌激素，含量为〈0．1％～36．27％。7种雌激素的检出率为39．14％～100．0％。结论 雌激素含量〉／1．0％的塑料玩具制品比重较大，其中DBP和DEHP检出率较高，应当引起重视。     

水中双酚A和烷基酚聚氧乙烯醚降解物的GC—MS测定方法研究

目的建立水中烷基酚聚氧乙烯醚（APEOs）降解物（NP、OP、NP1EO、NP2EO、OP1EO和OP2EO）和双酚A（BPA）的GC—MS检测方法。方法样品经盐酸酸化、二氯甲烷微液液萃取（micro-LLE）、浓缩、BSTFA硅烷化处理和正己烷定容后进行GC-MS分析。结果标准物浓度在10～200I~g／L范围内,本方法线性关系良好（R2度大于等于0．9992）;方法的检测限为1．39～5．34ng／L;加标（20和100ng／L）回收率为85％～105％,日间偏差小于等于6％;在2个月的饮用水监测实际应用中,内分泌干扰物（EDCs）检出率为100％,各个EDCs的暴露水平为0．5～90ng／L。结论该方法灵敏度高、选择性好、操作简单且成本较低,可以在常规实验室条件下满足水样中该类的分析要求。     

高效液相色谱法测定环境雌激素

本文研究了桶装饮用纯净水和河底淤泥中环境雌激素的高效液相色谱测定法。纯净水样品用固相萃取小柱浓缩净化，淤泥样品用甲醇—乙酸乙酯萃取，被测组分经五氟丙酸酐(PHA)衍生化后用高效液相色谱法进行定性、定量检测，检出限为0．1～1．0mg/L，被测组分的加标回收率为95．3％～106．6％。     

火焰原子吸收法采用锌灯同时测定水与食品中锌铜的研究

目的：介绍采用锌空心阴极灯同时测定水与食品中锌铜的方法，实现一灯多用的目的。方法：采用锌空心阴极灯波长（213．9nm）测定水与食品中锌，再把波长改变成铜的波长（324．8nm）其它测定条件不变，测定水与食品中铜。结果：通过实验，锌检出限（水：0．042mg／L、食品：0．10mg／kg），相对标准偏差（水：6．2％、食品：5．3％）、回收率（水：90．0％～95．0％、食品：92．0％～105．0％）、铜检出限（水：0．17mg／L、食品：0．076mg／kg），相对标准偏差（水：6．0％、食品：5．6％）回收率（水：94．0％～98．0％、食品：91．5％～96．2％）。结论：此法可减少灯的预热时间延长仪器的使用寿命，操作简便，快速，精密度和准确度都好，能满足水与食品中锌、铜的测定。     

腐竹中碱性嫩黄O和碱性橙Ⅱ测定方法探讨

目的建立1种同时测定腐竹中碱性嫩黄0和碱性橙Ⅱ的高效液相色谱方法。方法采用乙腈-水（7＋3）溶液对粉碎后的腐竹样品进行超声提取,在甲醇和乙酸铵水溶液梯度条件下进行洗脱,并在436nm波长下进行测定。结果该方法测定碱性嫩黄0和碱性橙Ⅱ在0．1～25．0μg／mL浓度范围内呈良好线性关系,相关系数分别为0．9992和0．9989,3个水平（5．0、10．0、15．0mg／kg）的加标回收率分别为89．5％～93．6％和90．5％～93．9％,相对标准偏差分别为0．50％-1．03％和1．12％～1．36％。检出限碱性橙Ⅱ为0．015mg／kg、碱性嫩黄0为0．010mg／kg。结论此方法具有简单、快速、准确等优点,适用于腐竹中碱性嫩黄0和碱性橙Ⅱ的同时测定。     

高效液相色谱法测定食品及保健品中维生素C含量的研究

目的：建立食品及保健食品中维生素C的高效液相色谱测定方法。方法：采用ODS C18柱分离；流动相为甲醇＋0．1％辛烷磺酸钠（7＋93）；流速1．00ml/min；二级管阵列检测器，检测波长230nm。结果：本方法线性范围为0．30～16．0μg／ml，加标回收率在97％～101．0％之间，RSD在0．56％～1．81％之间，方法检出限为0．301μg／ml。结论：该方法简便、快速、准确，适用于食品及保健食品中维生素C含量的测定。     

超高效液相色谱-串联质谱法测定奶茶中4种烷基酚类化合物

目的建立超高效液相色谱-串联质谱法测定奶茶中双酚A(BPA)、双酚S(BPS)、辛基酚(OP)和壬基酚(NP)的残留量。方法奶茶样品经过离心后,直接取上清液用固相萃取柱进行净化,然后用ZORBAX SB-Aq色谱柱(3. 0 mm×100 mm,1. 8μm)分离,再用甲醇和5 mmol/L乙酸铵溶液作为流动相进行梯度洗脱,最后注入到质谱仪中,以电喷雾负离子模式(ESI-)电离,多反应监测模式(MRM)进行检测。结果 BPA、BPS在2μg/L～100μg/L线性关系良好(r 0. 999),方法的检出限(S/N=3)为0. 3μg/L、0. 01μg/L,回收率为75. 0%～86. 7%,相对标准偏差(n=6)为1. 0%～5. 8%; OP、NP在10μg/L～500μg/L线性关系良好(r 0. 999),方法的检出限(S/N=3)为0. 7μg/L、0. 9μg/L,回收率为73. 4%～112. 0%,相对标准偏差(n=6)为1. 9%～5. 9%。结论该方法简单、灵敏、准确可靠,适用于奶茶中4种烷基酚的测定。     

离子色谱法测定食品中的甜蜜素和苯甲酸

目的：采用离子交换-电导检测离子色谱法测定食品中的甜蜜素和苯甲酸。方法：选用IonPacAS11-HC分析柱，25．0mmol／L NaOH＋5％甲醇淋洗液，外接水自动再生，样品经沉淀处理，过滤后进样分析。结果：方法的线性范围广、相关性好（r〉0．999），甜蜜素和苯甲酸样品及标准测定的相对标准偏差（RSD）分别为0．2％～4．8％、3．5％、0．1％～7．6％、0．6％，样品加标回收率分别为90．4％～105．1％、92．0％～106．8％，检出限分别为0．48、0．57mg／kg。结论：与国标方法对比测定的结果表明，该方法的准确度高，适用性较好。     

高效液相色谱-二极管阵列检测器法检测饮料中Vc的研究

目的：建立高效液相色谱（HPLC）-二极管阵列检测器（PDA）法测定饮料中Vc含量的检测方法，并探讨更确切的定性方法。方法：用0．01mol／L盐酸溶解稀释样品，经0．45μm滤膜过滤，以0．02mol／L乙酸铵-甲醇（7＋3）作流动相，采用Diamonsial C18柱分离，在比对保留时间的基础之上，对照样品与标准Vc的光谱形状、最大吸收波长等特征。结果：只有保留时间和光谱特征两项指标都符合才能确认，增强了定性的确定性。方法线性范围为1.0-40．0μg／ml，r=0．9998，加标回收率为97．5％-105％，RSD为2．1％-4．6％，检出限为0．5ng（S／N=3）。结论：该方法简便、快速，定性能力强，易于普及，适于食品中Vc的快速测定。     

高效液相色谱直接测定保健酒中的牛蒡苷

目的：研究高效液相色谱法直接测定保健酒中的牛蒡苷。方法：选择甲醇／水为流动相体系，流速0．8ml／min。结果：当检测波长为230nm时检出限为0．8ng，加标回收率为94．6％～105％，线性范围为0．025～5．0μg，相关系数为0．9998，相对标准偏差为1．07％；当检测波长为280nm时，检出限为3．0ng，加标回收率为99．2％～104％，线性范围为0．05～5．0μg，相关系数为0．9999，相对标准偏差为1．12％。结论：直接测定法方法简便、结果可靠、灵敏度高。     

Urinary concentrations of bisphenol A and 4-nonylphenol in a human reference population

Bisphenol A (BPA) is used to manufacture polycarbonate plastic and epoxy resins, which are used in baby bottles, as protective coatings on food containers, and for composites and sealants in dentistry. 4-Nonylphenol (NP) is used to make nonylphenol ethoxylates, nonionic surfactants applied as emulsifying, wetting, dispersing, or stabilizing agents in industrial, agricultural, and domestic consumer products. The potential for human exposure to BPA and NP is high because of their widespread use. We measured BPA and NP in archived urine samples from a reference population of 394 adults in the United States using isotope-dilution gas chromatography/mass spectrometry. The concentration ranges of BPA and NP were similar to those observed in other human populations. BPA was detected in 95% of the samples examined at concentrations > or = 0.1 microg/L urine; the geometric mean and median concentrations were 1.33 microg/L (1.36 microg/g creatinine) and 1.28 microg/L (1.32 microg/g creatinine), respectively; the 95th percentile concentration was 5.18 microg/L (7.95 microg/g creatinine). NP was detected in 51% of the samples examined > or = 0.1 microg/L. The median and 95th percentile concentrations were < 0.1 microg/L and 1.57 microg/L (1.39 microg/g creatinine), respectively. The frequent detection of BPA suggests widespread exposure to this compound in residents of the United States. The lower frequency of detection of NP than of BPA could be explained by a lower exposure of humans to NP, by different pharmacokinetic factors (i.e., absorption, distribution, metabolism, elimination), by the fact that 4-n-nonylphenol--the measured NP isomer--represents a small percentage of the NP used in commercial mixtures, or a combination of all of the above. Additional research is needed to determine the best urinary biomarker(s) to assess exposure to NP. Despite the sample population's nonrepresentativeness of the U.S. population (although sample weights were used to improve the extent to which the results represent the U.S. population) and relatively small size, this study provides the first reference range of human internal dose levels of BPA and NP in a demographically diverse human population.     

雌性大鼠血清和组织中壬基酚的高效液相色谱测定法

目的建立大鼠血清及组织样品中壬基酚(NP)的液-液萃取和高效液相色谱荧光检测方法。方法清洁级SD雌性大鼠血清采用正己烷-乙醚混合溶剂(V∶V=7∶3)提取,组织采用甲醇-乙酸铵缓冲液(pH值为4.5,V∶V=2∶8)提取,采用C18色谱柱分离,乙腈-乙酸铵缓冲液(pH值为4.5,V∶V=95∶5)为流动相,柱温40℃,在激发波长227nm,发射波长313nm处用荧光检测器检测。结果血清和组织中NP含量与峰面积呈良好的线性关系,线性范围为0.1～30.0μg/ml。检出限为13ng/ml,加标回收率为92.60%～108.00%,日内精密度RSD为0.29%～1.51%,日间精密度RSD为0.74%～1.57%,均小于2%。结论该方法简便易操作、灵敏准确,回收率好,精密度高,适用于动物血清及组织中环境雌激素NP含量的检测。     

Immunoaffinity columns and determination of ochratoxin A in cereals by HPLC. Part II. Evaluation of extraction using acetonitrile/water

Ochratoxin A from wheat and rye grain was extracted with acetonitrile:water (60:40). After clean-up of extracts using immunoaffinity columns (IAC), ochratoxin was determined by high-performance liquid chromatography using C18 column and fluorometric detection at 330 nm excitation and 460 nm emission. The mean recovery of ochratoxin A at fortification levels 0.1-100 microg/kg, was 74-89%. The limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.025 microg/kg, respectively. The positive results were confirmed by reaction with BF3 complex in methanol.     

Determination of clenbuterol in biological samples by high performance liquid chromatography with in series ultraviolet and electrochemical detection]

A method for the determination of clenbuterol in animal tissues and fluid is described. After a three-step pretreatment, involving sample extract, liquid-liquid partition and purification on a LC-WCX column, the separation of clenbuterol from interfering compounds present in biological samples was performed on a Hypersil BDS C18 column by high performance chromatography with in series ultraviolet and electrochemical detection. The mobile phase was a mixture of methanol and 0.01 mol/L potassium chloride (45:55). The UV-absorption 244 nm and the electrochemical detection pulse mode +1.0 V were applied in series. The results showed that concentration of clenbuterol and peak areas achieved a nice linear relation. The limit of detection of clenbuterol in animal foods is 0.5 microg/kg. The mean recovery of clenbuterol spiked at 2.5, 2.0, 1.5, 0.5 microg/kg levels with chicken and liver samples were 42.2%-96.1%, RSD were from 12.4 to 19.7% (n = 7). With the described method, animal food samples and biological fluid (e.g. urine and blood) were analyzed with satisfaction.     

反相高效液相色谱法测定罗哌卡因在犬血浆中的浓度

目的建立反相高效液相色谱法测定犬血浆罗哌卡因浓度的快速、简便的方法。方法色谱柱为Intertsil C18柱(4·6mm×250mm,5μm),流动相为甲醇-水相,体积比为50∶50,水相为0·005mol/L己烷基磺酸钠,冰醋酸调节pH至3·5,检测波长为215nm,流速为:1·4ml/min;柱温为室温;柱压为2800PSI,进样体积为10μl,灵敏度为0·02AUFS。结果罗哌卡因的检测浓度线性范围为0·1~25μg/ml(r=0·9992),最低检测浓度为0·05μg/ml,回归方程为^Y=0·1794X+0·3806,相关系数为r=0·9992,回收率为91·2%~93·6%,RSD为2·10%~3·40%。罗哌卡因测定的日内及日间精密度分别为1·35%~2·88%和1·80%~3·76%。结论本法操作简便、可靠、快捷、准确,适用于罗哌卡因类药物给药后血药浓度的检测。     

在线固相萃取-液相色谱串联质谱法测定饮用水中的双酚A和壬基酚

目的建立测定饮用水中双酚A(BPA)和壬基酚(NP)的在线固相萃取-液质联用法(On-line SPE LC-MS/MS)。方法水样经On-line SPE在线富集和净化,以甲醇-水为在线固相萃取流动相,流速2.0ml/min,采用沃特世Direct Connect HP XBridgeTMC18在线固相萃取柱(填料粒径10μm)进行在线固相萃取。以甲醇-0.1%氨水为分析流动相,流速0.4ml/min,采用沃特世UPLC BEH C18色谱柱进行分析。质谱检测器采用电喷雾电离源,以多反应监测(MRM)方式进行负离子监测,采用内标法对饮用水中的BPA和NP进行定量分析。结果该方法每个样品总耗时10min。BPA线性范围为5～1000ng/L,NP为10～5000ng/L,相关系数(r2>0.999)。BPA、NP的定量限(LOQ)分别为5和10ng/L,两种内分泌干扰物在3个加标水平下平均回收率为86.6%～105%,相对标准偏差3.11%～18.2%,日间精密度11.3%～13.2%。结论该方法实现了样品的自动化前处理,提高了分析效率,操作简单,灵敏度高,可用于饮用水中两种环境内分泌干扰物的痕量检测。     

蔬菜中内分泌干扰物4-壬基酚和双酚A的GC-MS检测方法研究

目的建立蔬菜中内分泌干扰物4-壬基酚(4-NP)和双酚A(BPA)的GC-MS检测方法。方法样品粉碎后,超声波振荡提取,BONDELUTCH固相萃取小柱净化,二氯甲烷洗脱,无水硫酸钠脱水后BSTFA衍生,GC-MS测定。结果两种目标化合物线性范围为10~500μg/L(r=0.999),4-NP和BPA的检出限分别为0.1μg/kg和0.02μg/kg,样品平均加标回收率为85.0%~105.1%,批内、批间精密度均小于10%。结论该方法具有良好的批内和批间精密度,灵敏度高,适用于蔬菜中痕量4-NP和BPA检测。     

Bisphenol A, 4-tert-Octylphenol,and 4-Nonylphenol in The Gulf of Gdańsk (Southern Baltic)

The organic derivatives of phenol are classed as dangerous compounds, and their presence has been detected in surface water, bottom water, phytoplankton, zooplankton, and mussel as well as liver and muscle of fish from the Gulf of Gdańsk and in liver, muscle, and guano of gulls residing in the coastal zone of this basin. The greatest sources of bisphenol A (BPA), 4-tert-octylphenol (OP), and 4-nonylphenol (NP) were found to be the Vistula River and the water purification plant in D?bogórze. In living organisms, concentrations of BPA, OP, and NP ranged between the limit of quantification and several hundred ng g^?1 dry weight (dw), and the highest concentrations were found for BPA. Prolonged alimentary exposure to BPA, OP, and NP in fish and birds was indicated by liver/muscle concentration ratios generally >1. The most influential factors on BPA and alkylphenol concentrations in the tissues of fishes and gulls were mainly diet and habitat. The study confirmed possible bioaccumulation in the food web. High BPA and NP concentrations in guano (≤2,700 and ≤300 ng g^?1 dw, respectively) indicated the ability of birds to detoxify and signalled the reintroduction of these compounds to seawater. Herring, flounder, and cod from the Southern Baltic are a safe food source for human consumption because their BPA and alkylphenol contents are low.     

高效液相色谱-荧光检测法测定大气细颗粒物(PM2.5〖KG-*5〗)中的双酚A

目的 建立大气细颗粒物(PM2.5)中双酚A 的高效液相色谱-荧光测定法,并用于成都市大气细颗粒物(PM2.5)中BPA的测定。方法 以玻璃纤维滤纸为滤料,用中流量PM2.5 采样器以100L/min的流速连续采样24h。滤纸样品经0.1%盐酸-甲醇超声提取后经C18小柱固相萃取,用0.1%氨水-甲醇洗脱,洗脱液调pH 2~3后,C18色谱柱(250mm×4.6mm,5μm)分离,荧光法检测(λex=227nm,λem=310nm)。结果 在0.001μg/ml~0.020μg/ml范围内回归方程为y=5.39×106x+5146,相关系数大于0.997;方法检出限为3.0×10-5μg/ml,定量限为1.1×10-4μg/ml,最低检出含量为200pg/m3(取样1/8分析),加标回收率为94.9%~104.8%,RSD为2.84%~9.23%。利用本法检测了20个成都市大气细颗粒物样品,测得双酚A含量范围在<200~4654pg/m3,平均含量为1455pg/m3。结论 本法灵敏度高,准确度好,检出限低,适用于大气中细颗粒物中双酚A的检测。成都市大气细颗粒物中双酚A的含量高于日美等发达国家以及我国北京、广州、香港,但低于印度的报道值。     

固相萃取-超高效液相色谱-串联质谱法测定生活饮用水中11种全氟化合物

目的建立固相萃取-超高效液相色谱串联质谱(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)同时测定生活饮用水中11种全氟化合物的方法。方法采用WAX固相萃取柱对生活饮用水样品中的目标物进行富集净化,5 mL甲醇和7 mL 0.1%氨水-甲醇溶液洗脱,洗脱液用氮气吹至近干,30%(V/V)甲醇水溶液定容至1 mL,UPLC-MS/MS进行测定。结果11种目标分析物在0.5~50μg/L范围内具有良好的线性关系,方法检出限和定量限分别为0.03~0.7 ng/L和0.5~3.0 ng/L,低、中、高浓度加标回收率分别为90.0%~122.3%、87.1%~130.0%和80.0%~113.7%,相对标准偏差分别为1.95%~8.59%、1.27%~9.08%和2.17%~10.51%(n=6)。结论该方法线性范围宽,方法检出限和定量限低,适用于我国生活饮用水中11种全氟化合物的测定和监测。