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分析化学

分析化学

北大核心

CSCD

CSTPCD

Chinese Journal of Analytical Chemistry
《分析化学》是中国化学会和中国科学院长春应用化学研究所共同主办的专业性学术期刊，主要报道我国分析化学创新性研究成果，反映国内外分析化学学科前沿和进展。本刊旨在为冶金、地质、化工、材料、农业、食品、药物、环境等领域从事研究测试的科技人员及高等院校相关专业的广大师生提供最新的分析化学的理论、方法和研究进展，促进学术交流和科技进步，为国家的经济建设服务。
  • 发文量：14537
  • 被引量：4674
  • H指数：3
  • 开始收录时间：1977(5)
  • CNKI综合因子：1.338
  • 维普期刊影响因子： 1.353
  • 万方期刊影响因子：1.47
  • 创刊时间：1972
  • 国内刊号/CN：22-1125/O6
    国际刊号/ISSN：0253-3820
  • 发行周期：月刊
    邮发代号：12-6
  • 主管单位：中国科学院长春应用化学研究所
    主办单位：中国化学会 中国科学院长春应用化学研究所
分析化学-联系信息
  • 主编：杨秀荣
  • 电话：0431-85262017
  • 邮箱：fxhx@ciac.ac.cn
  • 地址：长春市人民大街5625号
  • 邮编：130022
分析化学-获奖情况
  • • 1999获首届国家期刊奖
  • • 2000年获中国科学院优秀期刊特别奖
  • • 2001年入选中国期刊方阵“双高”期刊
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分析化学 >2021年第012期

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  • 摘要：A portable gas chromatograph-mass spectrometer (GC-MS) was developed based on a quadrupole ion trap (IT) mass analyzer and a low thermal mass GC. The portable GC-MS system, mainly composed of a sample system, a low thermal mass GC module, a GC-MS interface and a miniaturized ITMS system, has a dimension of 44 cm×36 cm×22 cm and weighs of 14 kg. The power consumption during sample analysis is about 100 W. The ITMS system has a mass range of mlz 15-550 and can give a mass resolution at full-width half-maximum (FWHM) of less than 0.5 amu at a high scan rate up to 10,000 amu/s. Furthermore, the ITMS system has the ability of performing three-stage tandem mass spectrometry. The performance of the portable GC-MS system was investigated by testing the volatile organic compounds (VOCs) standard including EPA TO 14 and EPA-624 by this system. The portable GC-MS system can be used for in situ analysis of hazard compounds in a variety of complex and harsh environments with portability, rapid response, low detection limit and high specificity.%将双曲面三维离子阱质谱技术与低热容气相色谱技术相结合,研制了便携式气相色谱-质谱联用仪(GC-MS).此仪器主要由进样系统、低热容气相色谱模块、气质接口以及小型化离子阱质谱模块等构成,其主机重量小于14 kg,体积为44 cm×36 cm×22 cm,功耗小于100W.该仪器中的离子阱质谱仪系统具有15～550 amu的质量范围,在全质量范围内质量分辨率优于0.5 amu(FWHM),最高扫描速率可达10000 amu/s,此系统还具有三级质谱分析功能.采用此便携式GC-MS分别测试环境标准样品EPA TO- 14和EPA 624,结果表明,仪器具有定性能力强、分析速度快、检测灵敏度高、功耗小以及便携性能优等特点,可对空气、水体、固态废弃物中的有毒有害物质进行现场分析和检测.
  • 摘要：The thermal desorption is an important method for the introduction of liquid and solid samples into an ion mobility spectrometer (IMS). There are the problems of recondensation or decomposition for detecting low-volatile or thermally unstable organic compounds. A rapid thermal desorption device coupled with IMS membrane was developed. A micro-heater and a thermocouple were used to control the temperature of desorption for improving the efficiency of sample introduction. The experiments were carried out for the detection of low-concentration melamine solution. The effect of heating parameters on IMS product ion peak was investigated. The results show that the sample can be concentrated and sample loss and pollution can be reduced by using a temperature controlled heater with a heating rate of 76 ℃/s up to the 230 ℃ which ensures the linear response and low limit of detection (lower than 0. 05 ng).%热解析是用于离子迁移率谱仪(IMS)的液体和固体样品进样的重要手段,但在检测高沸点或易分解有机物时,存在易重新凝结或过热分解的问题.本研究建立了一种与IMS半透膜结合的热解析进样方法,设计了可快速加热的微型热解析装置,通过热子通电发热及热电偶测温实现对样品解析区域的升温控制,提高半透膜的进样效率.以低浓度三聚氰胺溶液为例进行了检测实验,分析了解析装置的加热特性及不同温度和升温速度下的IMS产物离子峰变化.结果表明,采用升温速率为76℃/s的脉冲加热至230℃的热解析方法,样品释放集中,通过半透膜时损失和污染少,保证了输出线性和较低的检出限(低于0.05 ng).
  • 摘要：A dynamic stability technique for antomatic calibration of trace concentration of radon in the air and the method for the precise detection of the concentration of radon and radon decay products were tentatively investigated. A homemade standard radon chamber with the functions of autocontrol-ling radon concentration, temperature and humidity, formation and collection of aerosol, was constructed. Setting up a detective and experimental study platform for radon detection instrument calibration and calibration devices with a radon chamber of 4 m3. This also sveer asa sensitive analyzer for detction of the radon decay products in radioactive aerosol were carried out. The radon concentration detected by the device ranges from 370 Bq/m3 to 20000 Bq/m3 with the precision of 3%. The calibration time of the homemade standard radon chamber for a single point is 40 min and for a radon instrumentation was 7 h. Moreover, 3 active mode radon instruments and 4 to 6 passive mode radon instruments can be corrected simultaneously. The certificate, report, data and results can be automatically generated and saved, and the operators can find the results in many ways.%研究了空气中痕量氡的动态稳定技术和氡及其子体浓度的准确测量方法.研制了具有氡浓度自动控制、温湿度调控、气溶胶发生/采集等功能的标准氡室,并建立了主氡室标称体积达4 m3的氡测量仪器检定/校准装置和氡子体放射性气溶胶检测与实验研究平台.研究表明,本装置测氡浓度范围为370～20000 Bq/m3；检测精确度达3％；单点校正时间为40 min;单台仪器校正时间为7h,可同时进行3台主动式和4～6台被动式测氡仪的检定或校准,并能够按照检定/校准结果自动生成证书及报告,自动保存测量数据,且可以按多种方式进行查询.
  • 摘要：A novel High-performance liquid chromatographic method of determining monomer migration of melamine (MEL) and its derivatives including ammeline (ANE), ammelide (ADE) and cyanu-ric acid (CYA) was developed. Samples were immersed in simulants (H2O, 4% acetic acid, 10% ethanol), and then kept in incubator at 70 ℃ in a duration of 4 h. The immersed solutions were injected into HPLC column before the penetration through a 0. 45-μm microporous membrane. The separation was performed on a Phenomenex Luna NH2 column at 30 ℃ and the mobile phase of acetoni-trile (5 mmol/L) with PBS (pH =6. 5)(75:25, V/V) of isocratic elution was pumped at a flow rate of 1. 0 mL/min with DAD detection at 205 and 214 nm. Under the optimum conditions, the calibration curves were linear from 0. 5 to 10 mg/L with LODs (S/N = 3) of 0. 06, 0. 08, 0. 12 and 0. 15 mg/L for MEL, ANE, ADE and CYA, respectively. The method provided recoveries of 96. 4% - 101. 6% in the spiked concentration of 1. 0 mg/L, and the RSD of the peak height was between 2. 8% and 4. 4%. The satisfied experimental results indicated that the proposed method can be directly used for the determination of monomer migration of melamine and its derivatives in food contact material conveniently, rapidly and accurately.%建立了高效液相色谱同时检测三聚氰胺(MEL)及其衍生物——三聚氰酸二酰胺(ANE)、三聚氰酸一酰胺(ADE)和三聚氰酸(CYA)单体迁移量的方法.样品分别采用水、4％乙酸、10％乙醇作为食品模拟物,在70℃浸泡4h,浸泡液过0.45μm微孔薄膜后进入色谱柱.色谱分离采用Luna NH2柱,柱温:30℃,流动相为V(乙腈):V((5 mmol/L PBS缓冲溶液,pH 6.5)=75:25,流速:1.0 mL/min; DAD检测波长为205和214 nm.在此优化条件下,MEL,ANE,ADE和CYA的浓度在0.5～10 mg/L范围内与其峰面积的线性关系良好,检出限分别为0.06,0.08.0.12和0.15 mg/L(S/N=3).在1.0 mg/L的添加水平下,MEL,ANE,ADE和CYA的平均回收率在96.4％～101.6％之间,相对标准偏差在2.79％～4.39％之间.结果表明,本方法可简便、快速、准确地同时测定食品接触产品中三聚氰胺及其衍生物的迁移量.
  • 摘要：The characters and applications of combined single photon ionization (SPI) and photoelec-tron ionization (PEI) source were introduced. The ion source can generate dominated molecular ions in SPI mode and fragments ions same as standard El spectrum in PEI mode. The switch time between the two modes was several microseconds. The limit of detection in SPI mode was reduced by increasing the optical path in the ion source. Achieved detection limits were 0. 05 mL/m3 and 20 mL/m3 for benzene in SPI mode and SO2 in PEI mode with accumulating time of 4 s respectively. Products in the process for catalytic dehydrogenation of alkanes were monitored in SPI mode. In addition, the samples of SF6 were analyzed in PEI mode with low energy electrons and the impurities were identified.%复合电离源在单光子电离模式下可以产生分子离子信号,易于确定分子量；在光电子电离模式下,70 eV电子能量可以产生含有物质结构信息的碎片峰,实现物质的结构鉴定.两种电离模式可以实现毫秒级迅速切换.本研究通过提高光程降低了单光子电离模式下的检出限.在单光子电离模式下,对苯的检出限为50 μg/m3(累加时间为4s)；光电子电离模式下,对SO2的检出限为20 μL/m3(累加时间4 s).利用复合电离源的单光子电离模式分析了烷烃催化脱氢产物,成功实现了碳链长度为8～12的烷烃,烯烃和二烯烃的在线分析和监测.此外,还利用低能电子的光电子电离模式分析了高压变压器保护气,检测了主要杂质成分,为高压变压器中故障的快速诊断提供依据.
  • 摘要：研制了一种只用-10C低温的冷阱浓缩/热解析仪,用于大气中C2和C2以上挥发性有机物的在线检测.以碳分子筛TDX-01和石墨化炭黑为吸附剂,将大气挥发性有机物富集在吸附管内,通过对吸附管直接加热快速热解析后,样品随载气直接进入气相色谱仪进行分离分析,不需二级冷阱或者二次浓缩.对10种挥发性有机物的检测显示,测定结果的相对标准偏差均小于5％;线性相关系数均大于0.99;检出限为14×10-12～52×10 12(V/V).相比与传统的采用液氮或者半导体制冷为冷源的热解析仪,本装置具有结构简单,体积小巧,功耗低等优点,适用于对大气痕量挥发性有机物的准确、快速分析.%A cryogen-free refrigerating preconcentration/thermal desorption device that used a refrigeration compressor as cold source has been developed, optimized and characterized. Only -10 ℃ was needed to trap volatile organic compounds (VOCs) down to C2 in ambient air. The device was applied for the on-line determination of VOCs in ambient air. Carbon molecular sieves TD×-01 and graphi-tized carbon black were used as adsorbents for enrichment of VOCs at -10 ℃. The trapped analytes were thermally desorbed, and were directly transferred into the gas chromatography for analysis without any second cryotrap or secondary condensation. Experimental results showed that the relative standard deviations were less than 5%, the correlation coefficients were more than 0. 99, and the detection limits ranged from 14 × 10-12 - 52 × 10-12 (V/V) for 10 volatile organic compounds being tested. Compared with the traditional thermal desorption units that use liquid nitrogen or thermoelectric coolers as cold sources, device is more applicable for the rapid analysis of trace VOCs in air with merits of compactness, small size and low power consumption.
  • 摘要：建立了基于溶出伏安法的铋微阵列电极检测饮料中重金属的方法.该传感器采用三电极体系,铋微阵列电极为工作电极,铂薄膜电极为对电极,Ag/AgCl电极为参比电极.铋是一种低毒的重金属,采用铋作为反应物质可以使检测过程更加安全.微阵列电极具有高通量测定、便于微型化、抗干扰性等优点.实验表明,该传感器可同时检测出pb2+和Cd2+,检出限分别为0.067和0.064 mg/L,且具有很好的重复性.此传感器用于检测橙汁中的Pb2+和Cd2+,结果令人满意.%A heavy metal sensor fabricated by microelectronic mechanical system (MEMS) technology was described in this study. The sensor is three-electronic system which consisted of Bi microelectronic array working electrode, Pt counter electrode and Ag/AgCl reference electrode. Bi is low-toxic heavy metal, so the using of Bi as reaction substances can make detection process more safely. Microarray electrode takes many advantages, such as high-throughput, miniaturization and anti-interference. The experiment result shows that the sensor has a good performance in simultaneously detecting Pb2+ , Cd2+. The detection limits of these two metals are 0. 067 mg/L (Pb) and 0. 064mg/L (Cd) respectively with good repeatability. The sensor has been applied to detect Pb2+ (0.1 mg/L) and Cd2+ (0. 025 mg/L) in Orange juice with satisfactory results.
  • 摘要：1 引 言铋和锑是金锭中的主要杂质元素,依据国家金锭标准[1],铋和锑是必检项目.测试铋和锑的国家标准方法[2]不可同时测定,且检出限太高,对于高纯金锭无法做到精确测定.氢化物发生-原子荧光光谱法具有灵敏度高、检出限低、仪器相对便宜的优点,已广泛应用于冶金、地质和生物样品分析[3,4].本研究采用乙酸乙酯萃取-氢化物发生-原子荧光光谱法同时测定金锭中锑和铋的含量,检出限低,完全满足高纯金锭中铋和锑的含量分析.采用本方法对本公司高纯金锭样品进行加标回收实验,其结果与国家标准方法吻合.%A method was proposed for the simultaneous determination of antimony and bismuth in gold ingots by ethyl acetate extraction-hydride generation-atom fluorescence spectrometry. The detection limit of the method for bismuth and antimony was 0. 13 and 0. 012 mg/kg, respectively, the recovery rate was 92% - 97% and the relative standard deviations were below 1. 2%. The results indicated that the method is accurate with low detection limit. The analytical results were quite consistent with those by national standards method.
  • 摘要：A novel method for the separation and determination of trace cadmium in environmental water sample by flame atomic absorption spectrometry (FAAS) with ionic liquid extraction was proposed. When the acidity of the solvent was pH 8, ionic liquid 1-butyl-3-methylimi dazolium hexafluorophosphate ([Bmim]PF6) was used as extractant, dithizone as the chelant, the sample was extracted for 3 min and determined by FAAS. The research result indicated that under optimum conditions, there was favorable linearity relation between 0. 15 and 58. 2 μg/L, detection limit (3δ) was 0. 095 ng/L (n=11). The recovery of this method was in the range of 90. 0% -108. 0% . The relative standard deviation is less than 5. 8% for the analysis of practical sample.%1 引言化学工业排放的废水含有大量金属镉,对环境产生严重危害,因而环境水样中痕量镉的准确测定具有重要意义.目前,常用原子吸收光谱法[1]测定痕量的镉,但由于环境水样中镉的含量低且样品复杂,为了提高分析方法的灵敏度和选择性,样品的预分离与富集至关重要.液-液萃取是一种常用的预分离与富集方法,但常用有机溶剂作萃取剂,易带来二次污染.离子液体是一种无毒、无污染、不挥发的"绿色溶剂"[2],具有安全、高效、环保等优点[3],已萃取分离了多种金属离子[4-5].本实验以双硫腙(H2Dz)为螯合剂,以离子液体1-丁基-3-甲基咪唑六氟磷酸盐( [Bmim]PF6)为萃取剂.用火焰原子吸收光谱法(FAAS)测定了离子液体相中的Cd,建立了痕量Cd的分离与分析方法,并应用于环境水样的分析.
  • 摘要：A method based on cyclic voltammetry to modify the sensing surface to be macroporous copper nano-clusters was developed and for the detection of nitrate in a micro amperometric electrode, which was an electrochemical system composed of two-electrode system and fabricated based on Micro-Electro-Mechanical Systems (MEMS) technology. The experiment results demonstrate that this method as a controllable and convenient manipulation can effectively modify the surface of the working electrode for further nitrate determination more rapidly with less consumption of reagent, and enhance the sensitivity of the electrode. The experimental results reveal that under the optimal experimental conditions microelectrode surface modified by cyclic voltammetry electrodeposition was macro-porous and had a larger effective surface area, which shows marked sensitivity and selectivity for nitrate ions within the concentration range from 6. 25 to 3500 μmol/L (6. 25-300 μmol/L yielded straight lines: y1=- 0.0526x-3. 905,R12 =0. 9993, while in the range of 300-3500 μmol/L yielded straight lines: y2 = -0.0353x-13. 653,R22=0. 9918). Interference analysis with 9 kinds of ions (NO2- , Cl- , HPO42-/ P(V~ , SO42~ , HCOr/C(V~ , Na+ and K+ ) commonly found in groundwater indicates that only NO2-cause reasonable interference. These electrodes were applied to detect nitrate concentration in water samples from lake and river. The test results using these microelectrodes was consistent with the concentration given in the certificate of qualified water quality detection institute. This work is potential to develop a portable, cost-effective and accurate microsensor for real-time sensing of nitrate ions.%基于循环伏安扫描(CV)的电化学沉积方法制备出多孔性纳米簇状结构铜膜,结合采用微机电系统(Micro electro mechanical systems,MEMS)技术制备的微电极芯片,研制出用于NO-3;检测的安培型微传感器.考察该微传感器对NO-3;的响应性能,在6.25～300 μmol/L浓度范围内,灵敏度为0.0526 μA/(tmol/L),线性度99.93％；在300～3500 μmol/L浓度范围内,灵敏度为0.0353 μA/(μmol/L),线性度99.18％.与文献报道相比,该传感器表现出更高的灵敏度.考察水体中常见的NO-2,Cl-,HPO2-4/PO3-4,SO2-4,HCO3 /CO2-3,Na+和K+等离子对该传感器的干扰性能,传感器表现出较好的抗干扰性能.采用该微传感器对实际水样进行测试,测试结果与具有权威资质的测试公司的测试结果之间具有一定的相关性.实验结果表明,采用循环伏安沉积方法在微电极表面制备的纳米簇状结构的铜敏感膜,比表面积大,催化活性高,对NO;表现出了很好的敏感特性和选择性,适用于对微量NO3的检测.
  • 摘要：采用Fe3O4(核)/ZrO2(壳)纳米磁珠(ZMPs)标记待测物识别抗体,并用HRP酶封闭和DNA链接,建立了一类新型的“珠链状”一维磁性纳米探针制备方法.将甲胎蛋白(AFP)一抗固定于纳米金修饰的玻碳电极表面,构建了免疫电极(GCE ｜ AFP Ab1).基于该电极和上述合成探针,通过双抗体夹心法测定免疫产物上HRP酶对过氧化脲(CP)氧化对苯二酚反应的催化电流,研制了一类基于一维纳米结构组装的夹心型安培免疫传感器.研究表明:此一维纳米结构探针不仅大大增加了酶在电极表面的富集量,成倍扩增了催化电流,显著提高了传感器的灵敏度,而且易于通过外磁场与背景液可控分离,简化了分析步骤,并提高了结果的重复性.此传感器对AFP检测的线性范围为0.01～25tg/L;检出限达4 ng/L(3σ),并被用于人血清中痕量AFP的测定,结果满意.%A new type of one-dimensional magnetic nanoprobes was fabricated based on a DNA chain fixed with a number of Fe3O4 (core)/ZrO2 (shell) nano-magnetic beads (ZMPs) labeled with secondary antibody. The a-fetoprotein (AFP) was analyzed by using probes DNA/(ZMPs-HRP-AFP Ab2)n and immobilizing a-fetoprotein antibody (AFP Ab,) onto the glassy carbon electrode modified by nano-gold. The sandwich-type immunocomplex could be formed between the immobilized AFP Abi on the GCE and the probes DNA/( ZMPs-HRP-AFP Ab2) n and the carried HRP could catalyze the electrochemical reduction of carbamide peroxide (CP) with the help of hydroquinone (HQ). The novel one-dimensional nano structure assemble and sandwich-type amperometric immunosensor was developed. Enhanced sensitivity was achieved by introducing more HRP-AFP Ab2 onto the electrode surface through the pearl chain structure. Under optimal conditions, the proposed method could respond to 4 ng/L AFP with a linear calibration range from 0.01 to 25 ug/L. The immunosensor was employed to determine AFP in serum samples and the results were satisfactory. The proposed amperometric immunosensor was sensitive, quick, magnetic field controllable. This study provided a platform technology for developing a one-dimensional assembly and highly sensitive immunosensor, which was suitable for screen determination of tumors in serums of normal patients.
  • 摘要：制备了以二硫基琥珀酰亚胺丙酸酯,4-巯基苯硼酸功能化CdTe量子点探针,对其进行了X-射线光电子能谱和透射电镜表征.在431 nm激发波长下,对探针及加入多巴胺后进行发射光谱扫描,最大发射峰红移,在最大发射波长处,多巴胺对合成的探针具有猝灭效应,且多巴胺对体系的猝灭程度与多巴胺的量呈良好的线性关系,据此建立了一种直接、灵敏、选择性好的测定多巴胺的方法.在最佳条件下,多巴胺的其线性范围为0.02～20.0μmol/L,线性回归方程为ΔF=20.1+ 31.7C(μmol/L),相关系数为R2=0.987,检出限为4.9 nmol/L.本方法已成功用于多巴胺注射液、血清及尿样中多巴胺的测定,结果满意.%CdTe quantum dots probe with both 4-mercaptophenylboronic acid and dithiobis(succinimi-dylpropionate) was designed and functionalized, and characterized by XPS and TEM. Emission spectra of CdTe quantum dots probe and dopamine was scanned under 431 nm excitation wavelength. The maximum emission wavelength shift red. At the maximum emission wavelength, dopamine results in fluorescence quenching of the probe. A direct, selective, and sensitive strategy for the determination of dopamine was established. The effects of determination conditions were investigated. Under the optimal conditions, a good linearity (R2 =0. 987) was obtained between fluorescence intensity and dopamine concentration in the range of 0. 02 - 20. 0 μmol/L. The linear regression equation was △F= 20. L + 31.7C(μmol/L). The limit of detection was 0. 0049 μmol/L. The method has been successfully applied to determine dopamine in injection, serous and urine with satisfactory result.
  • 摘要：建立了同时测定葡萄酒中14种禁用食品添加剂的超高效液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)分析方法.采用UPLC BEH C18( 100 mm×2.1mm×1.7 μm)色谱柱,对流动相的组成、缓冲液离子强度及质谱的各种参数进行了优化.结果表明,流动相的离子强度对食品添加剂的质谱检测有重要影响,以含1 mmol/L甲酸铵-甲酸缓冲液(pH 3.9)-乙腈为流动相,梯度洗脱,柱温35℃,可以在6 min内完成14种食品添加剂的分离和检测.在ESI负离子模式下,采用选择离子监测方法进行测定时,除三氯蔗糖、日落黄和酸性红13的检出限分别为10,2和2 μg/L外,其它11种的检出限在0.01～ 1.0 μg/L之间.回收率为93.8％～106％,相对标准偏差小于3.1％.本方法快速、准确、灵敏度高,可用于葡萄酒及其它复杂基质食品中的低剂量、多种禁用食品添加剂的同时筛查.%An ultra performance liquid chromatography-eiectrospray ionization-tandem mass spectro-metric (UPLC-ESI-MS/MS) method for the simultaneous screening 14 illegal food additives (acesul-fame, sodium saccharin, sodium cyclamate, aspartame, neotame, sucralose, ponceau 2R, ponceau 3R, ponceau SX, sunset yellow FCF, allura red, acid Red 1, acid red 13, erythrosine) in wines has been developed. The HPLC separation was carried out using an UPLC BEH C18(100 mm×2. 1 mm× 1. 7 μm) as solid phase. Several parameters, including the compositions and ion strength of the mobile phase, and the monitor ions were optimized for improving the chromatographic performance and the sensitivity. The results demonstrated that the sensitivity could be significantly influenced by the amine concentration in the eluent. The separation could be completed in less than 6 min when using 1 mmol/L ammonium formate-formic acid buffer (pH 3. 9) and acetonitrile as the mobile phases, gradient elution. The column temperature was kept at 35 °C. When the analytes were detected by ESI~-MS under selected ion monitoring mode, the detection limits were 0. 01 - 1. 0 μg/L except sucralose, sunset yellow FCF, acid red 13 which were 10, 2 and 2 μg/L, respectively. The average recoveries ranged from 93. 8% to 106%. The relative standard deviations were less than 3. 1%. This method is rapid, accurate, highly sensitive and suitable for the quality control of low concentration and mixtures of food additives which were illegally added to wines and other foods.
  • 摘要：An ultra high performance liquid chromatography-tandem mass spectrometric method was established for the simultaneous determination of the residues of six industrial dyes in foods. The samples were extracted with 50 mmol/L ammonium acetate solution containing 50% methanol and 1% formic acid, cleaned up by WAX solid phase extraction column, and then analyzed in multiple reaction monitoring (MRM) mode. Sample matrix-matched calibration was used to determine the residue contents by external standard. Orange Ⅱ was detected with negative ion model, and the other five dyes were detected with positive ion model. Limit of quantitation (LOQ) of Chrysoidine Ⅱ , Rho-damine B , Auramine O , Rhodamine 6G and Safranine T was 1. 6 ug/kg,and LOQ of orange II was 6.0 ug/kg. The linear range of chrysoidine Ⅱ, rhodamine B, auramine O, rhodamine 6G and safranine T was 1. 0-100. 0 μg/L and that of orange Ⅱ was 5. 0-100. 0 μg/L, the linear correlation coefficients were all more than 0. 999. The recoveries of 6 dyes ranged from 70. 3% to 109. 2% with relative standard deviations (RSD) of 2. 6% -14.1%. This method was simple, effective and sensitive, and was suitable for the determination and confirmation of six industrial dyes added in the foods illegally.%建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测食品中6种工业染料含量的方法.样品用含50％甲醇和1％甲酸的50 mmol/L乙酸铵溶液进行提取、WAX弱阴离子交换固相萃取柱进行净化后,采用多反应监测(MRM)模式进行检测,基质曲线外标法定量.其中酸性橙Ⅱ采用负离子模式检测,其余5种染料采用正离子模式检测.碱性橙Ⅱ、罗丹明B、碱性嫩黄O、罗丹明6G、碱性桃红T的定量限为1.6 μg/kg,酸性橙Ⅱ为6.0 μg/kg;碱性橙Ⅱ、罗丹明B、碱性嫩黄O、罗丹明6G、碱性桃红T的线性范围为1.0～100.0 μg/L;酸性橙Ⅱ的线性范围为5.0～100μg/L,线性相关系数均大于0.999.6种染料的回收率为70.3％～109.2％；相对标准偏差(RSD)为2.6％～14.1％.本方法灵敏度高,操作简单高效,适合于食品中6种非法添加工业染料的定量及确证分析.
  • 摘要：Taking genotypes 10-11, 11-11, 10-12 and 10-13 of short tandem repeat (STR) locus D16S539 commonly used in forensic medicine as study objects, an ANN genotyping method was developed based on ultraviolet spectra of the measured samples and another ANN was used to extract the variables of rich information. Under the optimal conditions, each of the genotypes was amplified. The ultraviolet spectra of the samples that were produced by polymerase chain reaction, which was measured at length range of 200 - 310 nm, were pretreated and optimized by coupled ANN-ANN. The results showed that the best network structures of the rich information extraction ANN and the discriminant model built ANN were 391-50-391 and 50-6-4, respectively. The root mean square error for the training and the prediction samples sets was obtained to be 0. 0279 and 0. 0418. It was indicated that the models had a good ability of the robustness and big discriminating power for the prediction samples (the accuracy was 100%). The detection of STR genotypes by UVS was rapid, simple and low-cost.%以STR基因座D16S539中的总核心重复串数相差较小的10-11,10-12,11-11和10-13基因型为研究对象,以紫外光谱为判别变量,建立了以人工神经网络(ANN)提取富信息变量为基础的ANN基因分型方法.在优化条件下,对4个基因型样本进行了聚合酶链式反应扩增,以扩增样本在200～310 nm范围内的检测光谱进行预处理和偶合的ANN-ANN网络优化.结果表明,提取富信息变量和基因分型的ANN的最优网络结构分别为391-50-391和50-6-4,该结构下的判别模型的校正相对均方根误差(RMS)和预测RMS分别是0.0279和0.0418,模型表现出了良好的稳健性和100％的基因型正确预测率.成功实现了基于紫外光谱对STR基因型的快速、简单和低成本检测.
  • 摘要：The comparison and attribution analysis of volatile oil in Houttuynia cordata injection from pilot production and the corresponding herb were conducted, after the combination of multicomponent spectral correlative chromatography and chemometric resolution technique, based on the two-dimensional data from hyphenated chromatography GC-MS. The results showed that there were only 5 non-related Peaks among 40 Peaks of the injection and herb spectrochromatograms. That is, although the concentration of a large number of components fluctuated during the injection production process, most of ingredients in finished product injection came from the raw material herb. Only a very small number of components disappeared and occurred.%利用GC-MS提供的二维化学数据信息,通过多组分波谱相关色谱方法及化学计量学分辨技术,对中试生产的鱼腥草注射液及其对应的药材挥发性成分进行比较和归属分析.结果表明,在药材和注射液图谱的40个峰族中,只有5个非相关峰族,即在药材制成成品注射液过程中,尽管大量组分出现了浓度消长的现象,但是成品注射液的绝大部分成分来自药材,其中仅有少数组分出现了消失和生成现象.
  • 摘要：A method was developed for the simultaneous determination of iodide, thiocyanate and glyphosate in drinking water by capillary ion chromatography (CIC). The sample was directly injected into CIC after filtrated by 0. 22 μm nylon filter membrane, and then analyzed by IC. The analytical column was Dionex IonPac AS19 (250 mm×0. 4 mm) and gradient KOH was used as the eluent at a flow rate of 1. 0 mL/min. The detection was performed by a suppressed conductive detector. The external standard calibration curve was used for the quantitative analysis. The linear range of the method for iodide, thiocyanate and glyphosate was 2. 0-100 μg/L, the correlation coefficients were 0. 9997, 0. 9998 and 0. 9998, and the detection limits (S/N=3) were 0. 3, 0. 2 and 0. 2 μg/L, respectively. The average recoveries were 86. 0% -100. 6%. The method has been applied to determine trace iodide, thiocyanate and glyphosate in bottled drinking water with satisfactory results.%建立了一种采用毛细管离子色谱法同时测定饮用水中痕量碘离子(I-),硫氰酸跟(SCN-)和草甘膦(Glyphosate)的方法.样品经过0.22μm滤膜过滤后,直接进样5 μL,采用IonPac AS19(250 mm×0.4 mm)毛细管色谱柱分离,KOH梯度淋洗,流速10μL/min,抑制电导检测,外标法定量.以信噪比S/N=3计算检出限,I-,SCN-和草甘膦的检出限分别为0.3,0.2和0.2 μg/L,线性范围2.0～100 μg/L,相关系数分别为0.9997,0.9998和0.9998,加标回收率为86.0％～100.6％.本方法应用于饮用水中痕量I-,SCN-和草甘膦的测定,结果令人满意.
  • 摘要：Three pyrethroids (bifenthrin, cypermethrin and deltamethrin) in soil were determined by hollow fiber liquid-phase microextraction (HF-LPME) coupled gas chromatography-mass spectrometry (GC-MS). The sample preparation and extraction conditions were optimized, and the optimum conditions obtained as follows; ratio of soil to water was 1:3, pH value was 4, ultrasonic time was 5 min, extraction solvent was cyclohexane, extraction temperature was 25 ℃ , stirring speed was 900 r/min, and extraction time was 20 min. After extraction, 1 μL organic solvent was introduced to GC/MS for analysis. Under the optimize condition, using selected ion mode (SIM), the linear range for bifenthrin, cypermethrin and deltamethrin was 0. 01 - 25 mg/kg, 0. 5 - 50 mg/kg and 0. 5-50 mg/kg, respectively. The limits of detection (LOD) were 0. 003, 0. 020 and 0. 040 mg/kg, and the relative standard deviations(RSD) were 4. 3%, 4. 7% and 8. 6%. The results demonstrated that the method was feasible for the determination of pyrethroids in soil.%采用中空纤维膜-液相微萃取-气相色谱/质谱法测定土壤中3种拟除虫菊酯类农药(联苯菊酯、氯氰菊酯、溴氰菊酯).实验优化的样品制备和萃取条件为:土壤与水的质量比为1:3,pH=4,超声时间为5 min,萃取剂为环己烷,萃取温度为25℃,搅拌速率为900 r/min,萃取时间为20 min.萃取后取1 μL萃取剂进行色谱分析.在此条件下,当采用SIM模式时,测得土壤中联苯菊酯、氯氰菊酯和溴氰菊酯的线性范围分别为0.01～25 mg/kg,0.5～50 mg/kg和0.5～50 mg/kg;检出限分别为0.003,0.020和0.040 mg/kg;相对标准偏差分别为4.3％,4.7％和8.6％.本方法可用于土壤中拟除虫菊酯类物质的快速测定.
  • 摘要：A fluorescent silica nanobead-based immunochromatographic test strip was developed for the rapid and quantitative detection of clenbuterol (CLE). An orthogonal L9(3)3 test was designed, various parameters including amount of anti-CLE monoclonal antibody (mAb) used for nanobeads labeling, mAb labeled beads on conjugate pad, and antigen amount on test line were investigated and optimized. Under the optimal conditions, the linear range was from 0. 28 to 3. 3 μg/L. The recoveries of CLE spiked in swine urine were between 81. 7% and 101%. The results demonstrated that this test strip can be used for rapid, sensitive and quantitative detection of CLE in swine urine.%采用荧光硅球为标记物制备了快速定量检测克伦特罗(CLE)的荧光硅球免疫层析试纸条.通过正交实验得到最优荧光硅球抗体标记量、硅球垫抗体标记物用量以及检测线抗原浓度.在最优条件下,试纸条线性范围为0.28～3.3μg/L.猪尿样品CLE加标回收率为81.7％～101％,表明此试纸条可实现猪尿中CLE残留的快速定量检测.
  • 摘要：A simple, rapid sensitive and accurate ultra performance liquid chromatography tandem mass spectrometry (UPLOMS/MS) method was developed for the simultaneous determination of five currently used herbicides in soil. The sample preparation using the modified QuEChERS (quick, easy, cheap, effective, rigged, and safe) method completed the extraction and clean-up steps in one procedure. In this none buffer QuEChERS method, samples were extracted with acetonitrile, cleaned up with primary secondary amine (PSA) and C18 sorbent, then centrifugated and filtrated before detection. The pretreatment method was simple, rapid and effective and can meet the detection requirements. The UPLC-MS/MS method was performed on Waters ACQUITY UPLCM BEH C18 (50 mm×2. 1 mm I. D. , 1. 7 μm) and the column temperature was 30 ℃, the gradient elution with methanol and pure water as the mobile phase and the flow rate was 0. 25 mL/min. The positive elec-trospray ionization (ESI+) source under the multiple reaction monitoring (MRM) mode and external standard method were used for quantification. The results showed that the correlation coefficients up to 0. 9984 were obtained across a concentration range of 0. 5 - 200 μg/L. The limits of detection (LOD) ranged 0. 005 - 0. 020 μg/kg (S/N=3), the limits of quantification (LOQ) were 0. 017 -0.067 μg/kg (S/N= 10). The method was validated with soil samples spiked at two fortification levels (4 μg/kg and 40 μg/kg) and recoveries were in the range of 75. 4% - 98. 5% with relative standard deviations (RSD) of 3. 2%-11. 8%.%建立了超高效液相色谱串联质谱法(UPLC-MS/MS)简单、快速、灵敏、准确地同时测定土壤中5种常用除草剂多残留量的方法.样品经改进的QuEChERS(快速、简单、廉价、高效、灵活和安全)方法一步完成萃取净化,未使用缓冲盐溶液,经乙腈萃取,N-丙基乙二胺(PSA)和C18吸附剂填料净化,离心后直接过膜上机检测,萃取和净化的效果满足检测要求.UPLC-MS/MS方法采用Waters ACQUITY UPLCTM BEH C18 (50 mm×2.1 mmi.d,1.7μm)色谱柱,柱温30℃,流动相为甲醇和水,梯度洗脱,流速0.25 mL/min,电喷雾电离源正离子(ESI+)多反应监测(MRM)模式检测,外标法定量.5种常用除草剂在0.5～200 μg/L范围内线性关系良好,相关系数为0.9947～0.9984.在4和40μg/kg水平下的平均加标回收率为75.4％～98.5％；相对标准偏差为3.2％～11.8％；方法的检出限(S/N=3)为0.005～0.020 μg/kg,定量限(S/N=10)为0.017～0.067 μg/kg.
  • 摘要：Stir bar sorptive extraction (SBSE) is a novel sample pretreatment method. Compared with solid phase microextraction, it has a larger solid phase volume and a higher extraction capacity. It can enrich analytes during self-stirring without an additional stirrer, which may cause competitive adsorption. So it has been widely used for pretreatment in food, environmental and biological samples. In this review, the recent research of stir bar sorptive extraction was summarized, including operating principle, novel coatings, novel extraction methods and the application of SBSE technique. The deficiency of SBSE was discussed and the development trend was also prospected.%搅拌棒吸附萃取是一种新型的固相微萃取样品前处理技术,具有固定相体积大、萃取容量高、无需外加搅拌子、可避免竞争性吸附、能在自身搅拌的同时实现萃取富集等优点,广泛应用于食品、环境和生物样品分析的前处理.本文综述了搅拌棒吸附技术的最新应用进展,重点阐述了新型搅拌棒吸附萃取涂层的研制、新型萃取装置的发展以及搅拌棒吸附萃取技术的应用现状,并探讨了搅拌棒吸附萃取存在的不足,展望了搅拌棒吸附萃取技术的发展趋势.
  • 摘要：利用阳离子型聚合物聚二烯丙基二甲基氯化铵(PDDA)和功能化的带负电荷的多壁碳纳米管(MWNTs)及石墨烯(GR)之间的静电吸附,通过层层自组装的方法在玻碳电极的表面制备了均一、稳定的(PDDA/GR/PDDA/MWNTs)5多层膜.以交流阻抗及循环伏安等方法对修饰电极的性质进行了表征.结果表明,该电极对过氧化氢(H2O2)的氧化显示出较好的电催化活性,在工作电位为1.0 V,0.067 mol/L磷酸盐缓冲溶液(PBS)中对H2 O2响应灵敏度高,检测范围宽,测定H2 O2的线性范围为6×10-6～1.4× 10-2mol/L(相关系数为0.997).检出限为1.2×10- 7mol/L(S/N=3).并且表现出良好的稳定性和高选择性.该电极用于实际样品中H2 O2的测定,结果令人满意.%An uniform stable poly(diallyldimethyl-ammonium chloride/graphene(PDDA/GR)/PDDA/ MWNTs composite membrane on the glassy carbon electrode were prepared by using layer-by-layer self assembly method based on the electrostatic adhesion among the cationic polymer PDDA and the functional negatively charged MWNTs and GR. The properties of the modified electrode have been studied by EIS and CV. The results indicate that this electrode shows better electrocatalytic activity in oxidation of H2O2. When working potential is set at 1.0 V, the electrode shows high sensitivity and wide detection range for detection of H2O2 in 0. 067 mol/L phosphate buffer solution. The range of linearity is 6×10-6-1.4 ×10-2 mol/L, the detection limit is 1. 2×10-7 mol/L (S/N = 3) and the linear correlation coefficient R = 0. 997. This electrode is of good stability and high selectivity.
  • 摘要：A reliable cell quenching and metabolite extraction method was crucial for microhial metabolism analysis. For metabolism analysis of Vibrio parahaemolyticus, liquid nitrogen and 75 % methanol (-80 ℃ ) were compared for their efficiency of cell quenching, and six different extraction solvents based on (I) chloroform, (ii) 75% cold methanol. (iii) water, (iv) methanol: chloroform; watcr=10:3:1 (V/V) , (v) methanol: chloroform: water = 3 = 1 = 1 (V/V) and (vi) methanol : chloroform = 1:1 (V/V) were compared for their efficiency of metabolites extracting., The metabolites were detected by GC-MS. The results showed that leakage of metabolite occurred when quenched with 75% methanol ( - 80 t); however this phenomenon did not occur with liquid nitrogen. 47 metabolites were found when extracted with 75% cold methanol, and the relative standard deviation of peak area was 8. 0%. In contrast, 40 or less metabolites were detected with other extraction methods, and the reproducibilities of those methods were unsatisfactory. For global analysis, quenching with liquid nitrogen and extraction with 75% cold methanol was very suitable for metabolomics studies of Vibrio parahaemolyticus.%以气相色谱-质谱联用(GC-MS)为分析方法,比较了液氮和75％甲醇(-80℃)两种溶液对副溶血性弧菌细胞的猝灭效果,以及氯仿、75％冰甲醇、水、甲醇-氯仿-水(10∶3∶1,V/V)、甲醇-氯仿-水(3∶1∶1,V/V)、甲醇-氯仿(1∶1,V/V)6种提取剂对副溶血性弧菌代谢物组的提取效果.结果表明,用75％甲醇(-80℃)猝灭副溶血性弧菌时,出现了代谢物泄漏现象,而液氮猝灭则不存在这个现象；检索发现,采用75％冰甲醇提取获得了47种代谢物,峰面积标准偏差为8.02％,其它5种提取剂获得代谢物种类少于40种,且重现性差.比较色谱峰数量、面积和重现性后发现,液氮猝灭、75％冰甲醇提取适于副溶血性弧菌代谢物组提取.
  • 摘要：A new method has been proposed for fast determination of hexafluorophosphate (PF6-) and some inorganic anions (F- , Cl- , NO3-, SO42- ). It was accomplished by valve switching between anion exchange guard column and separation column connected in series. With strong retentive ion (PF6-) only through guard column and the inorganic anions through both guard column and separation column, the separation was completed within a much shorter time. Under the optimum conditions, the linear ranges of the method for PF6-, F-, Cl- , NO3- and SO42- were 1 - 200 mg/L 0=0. 9997), 0. 1-25 mg/L (r=0. 9995), 0. 1-5 mg/L(r=0. 9997), 0.1 - 5 mg/L(r=0. 9997) and 0. 1 - 5 mg/L(r=0. 9999), whereas detection limits calculated at S/N = 3 were 8. 90, 0. 41, 0. 44, 1.23 and 1. 20 μg/L, respectively. The recoveries were in the range of 86. 5% -112. 2% with the relative standard deviations of 1. 4% - 4. 1%. The method could be applied to determine strong retentive and weak retentive ions simultaneously.%建立了快速测定离子液体中六氟磷酸根(PF6-)及其它常规阴离子(F-,C1-,NO-3,SO2-4)的离子色谱阀切换方法.通过保护柱与分离柱的简单切换,使强保留离子PF6-仅通过保护柱,缩短其流通路径,在较短时间内出峰,其它离子既通过保护柱又通过分离柱,从而达到快速同时分离的目的.样品经稀释溶解后直接进样,淋洗液选用KOH,流速为1.0 mL/min,采用抑制型电导检测,外标法定量.PF6 -,F-,Cl-,NO3-和SO4-2的线性范围分别为1～200 mg/L,0.1～25 mg/L,0.1～5 mg/L,0.1～5 mg/L和0.1～5 mg/L,线性相关系数均大于0.9995；加标回收率在86.5％～112.2％之间；相对标准偏差在1.4％～4.1％之间,检出限分别为8.9,0.41,0.44,1.2和1.2 μg/L.本方法适用于一系列强弱保留离子同时分析的问题.
  • 摘要：A self-made graphite probe direct sampling insertion device (DSD with an inductively coupled plasma mass spectrometry (ICP-MS) was used to measure the isotopic ratios of 240Pu/239Pu under the interference of uranium. The interferences of 238U to 239Pu and 240Pu were decreased because the uranium and plutonium in the sample could be separated on-line according to the evaporating discrimination on DSI of different element. The results of isotopic ratio obtained by DSI-ICP-MS are well consistent with the reference data and better than the results obtained by conventional solution nublizing sampling mode coupled with ICP-MS when the uranium is over 105 higher than the plutonium in the sample. The method of DSI-ICP-MS can be used in the isotopic ratio of plutonium measurement under the serious interference of uranium.%采用自制的石墨探针直接进样装置( DSI)与电感耦合等离子体质谱(ICP-MS)联用进行了强铀干扰下超微量钚同位素比的分析技术研究.实验结果表明,由于DSI分析中存在显著的铀钚的分馏效应,可以实现分析中铀、钚的在线分离,从而降低了238U强峰对239Pu和240pu分析的干扰.当样品中238U与239pu的原子数之比超过105量级时,用DSI-ICP-MS方法测得的钚的同位素比结果与参考值的相对偏差小于1％,明显优于常规的ICP-MS分析方法.本方法可用于铀材料中超微量钚同位素比的分析,以在一定程度上降低对化学分离的要求,从而减小化学分离的难度和工作量.
  • 摘要：癌基因C-myc激活和突变在胃癌形成过程中起着重要作用.通过毛细管电泳(CE)方法检测50例胃癌患者中C-myc基因突变,建立一种准确、快速诊断早期胃癌的方法.本实验采用PCR扩增胃癌及癌旁正常组织中C-myc基因第二外显子易发突变的部位基因序列,扩增样品分别经96℃变性和EcoRV酶切处理,以PAGE-SSCP,CE-SSCP,CE-RFLP分别对其突变情况进行检测.优化的CE检测条件:筛分介质PEO浓度3.0％,pH 8.2,电压15 kV,温度15℃；荧光检测:λex=488 nm,λem=520 nm.检测结果:C-myc基因总突变率为20.0％ (10/50).测序分析结果显示C-myc基因第二外显子第53密码子存在点突变,碱基A变为碱基T(GAT→GTT),碱基的改变使氨基酸由亮氨酸替代为谷氨酰胺.本研究数据证实C-myc基因突变与胃癌的形成紧密相关,CE检测C-myc突变基因可作为胃癌早期诊断的简便可靠的方法.%Activation of C-myc oncogene by mutation has been reported to play an important role in gastric cancer tumorigenesis. We determined C-myc mutation in 50 patients with gastric cancer by capillary electrophoresis (CE) to establish an exactly and volant clinical diagnostic method in early gastric cancer. In this experiment, genomic DNA was extracted from normal tissue and gastric cancer tissue and the sequence of C-myc oncogene on exon 2 (possible with high mutation frequency) in the extracted genomic DNA was amplified by polymerase chain reaction (PCR). Then amplified DNA samples were denatured at 96 oC and digested by EcoRV and detected by PAGE-single strand conformation polymorphism (SSCP), CE-SSCP, CE-restriction fragment length polymorphism (RFLP). The optimum CE detection conditions including 3. 0% sieving medium poly(ethylene oxide) (PEO), pH 8. 2, separation voltage of 15 kV and temperature of 15 oC were adopted. The laser-induced fluorescence detector was set at λex = 488 nm, λem = 520 nm. The results reveal that the mutation frequency of C-myc gene is 20. 0% (10/50). Sequence analysis further identified a point mutation of A to T in exon 2 codon 53 (GAT→GTT), causing an amino acid substitution of leucine to glutamine. This study may suggest a correlation of the mutation of C-myc oncogene with gastric cancer progression. This work also demonstrates that CE can offer a convenient and reliable method to early diagnosis of gastric cancer.
  • 摘要：A method for the simultaneous determination of seven adulterants including fenfluramine, pseudoephedrine, norpseudoephedrine, amfepramone, sibutramine, sildenafil and strychnine in slimming functional foods has been established. A mixture of 20 mmol/L sodium tetraborate-10 mmol/L SDS-5% acetonitrile was used as running buffer (pH 9. 0). The samples were analyzed by high performance capillary elctrophoresis under conditions of 17 kV; 25℃ with the detection wavelength of 195 nm. The upper limits of linear ranges were all 100 mg/L with linear correlation coefficients greater than 0. 998. The RSDs were 4. 5%-7. 9% (n = 7). The average recoveries were 79. 6% -112. 0%. The detection limits (S/N=3) were 0. 16 - 0. 65 mg/L. The method is simple, fast, sensitive, accurate, low cost and has been successfully applied to the determination of the 7 target chemicals in the slimming functional foods.%建立了同时测定减肥类功能食品中违禁成分芬氟拉明、伪麻黄碱、去甲伪麻黄碱、安非拉酮、西布曲明、西地那非和士的宁的高效毛细管电泳分析方法.以20 mmol/L硼砂-10 mmol/L SDS-5％乙腈溶液(pH 9.0)为运行缓冲液,在25℃,17 kV条件下测定,检测波长为195 nm.各待测物线性范围上限均为100 mg/L,线性相关系数均大于0.998,相对标准偏差为4.5％～7.9％(n=7)；平均加标回收率为79.6％～112.0％；检出限(S/N=3)为0.16～0.65 mg/L.本方法简便快速、灵敏准确、分析成本低,已成功应用于功能食品中上述减肥类违禁添加成分的测定.
  • 摘要：研究了卷烟辅材参数与有害成分释放量的关系.这些有害成分包括焦油、烟碱、CO、HCN、苯并[a]芘(B[a]P)、4-(甲基亚硝胺基)-1-(3-吡啶基)-1-丁酮(NNK)、巴豆醛、苯酚和NH3.使用多元校正分析,模型传递等化学计量学方法,对实验数据进行分析,建立了多元线性和多项式模型,通过独立验证样品和t检验确立了每种有害成分的最优模型；分析了各项辅材参数对有害成分释放量的影响权重.%This paper presented a systematic investigation into the relationship between the properties of cigarette auxiliary materials and the amounts of the harmful components in the mainstream smoke, including tar, nicotine, CO, HCN, benzo[a]pyrene (B[a]P), 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), Crotonaldehyde, phenol, and NH3. We employed several chemometric methods to build, transfer and validate the multivariate models, and established the best model for each of the harmful components. We also investigated the impact of every auxiliary material on the release of the harmful components into the mainstream smoke, and obtained consistent results with corresponding conclusions in tobacco research. The investigation is not only beneficial to the manufacture of low harm cigarette, but also helps the data analysis protocol in tobacco industry.
  • 摘要：用水基标样替代油基标样,建立X射线荧光光谱测定石油及其产品中微量元素含量的方法.以钒、锰、铁、镍为研究对象,采用乳化技术制备试样,用乳化剂司班80将水基标样和油结合起来,合成油包水型乳状液；采用理论a影响系数法和内标法校准油水差异校正基体效应.实验发现,如果基体组成已知,理论a影响系数法可以校正水基和油基的基体差异,水基标样和油基标样可直接互换；如果基体组成未知,采用内标法校正基体效应,需要将样品合成油水混合液校正才能成功.用原油和燃料油样品进行对比实验,测得结果与标准方法一致.%In the field of oil analysis by X-ray fluorescence spectrometry, a method was developed on basis of water-based standard sample instead of oil-based standard sample. Selecting the elements of vanadium, iron, nickel and manganese as the research objects, emulsification technology was applied to synthesize oil-water mixture in sample preparation and water-based standard sample and blank oil synthesized water-in-oil emulsion with emulsifier span80. The matrix effect was corrected by theoretical a influence coefficients or internal standard method. It was found that when the matrix composition of oil-base sample or water-base sample was known, the matrix effect was corrected by theoretical a influence coefficients, calibration samples of oil-base or water-base could be exchanged, and when the matrix composition was unknown, the matrix effect was corrected by internal standard method, but only synthesized oil-water mixture, calibration to be successful. Accuracy of the method was verified by comparison test of crude oil and fuel oil samples, the method was compared with the standard method, both test results were consistent.

    分析化学的期刊信息

    • 曾用名：
    • 创刊时间：1972
    • 地区：CHINA MAINLAND
    • 语言：中文
    • 热门主题：中国化学会;中国科学院长春应用化学研究所
    • 学科分类： 化学、晶体学;

      3

      CHEMISTRY, ANALYTICAL:Q4;

      Chemistry:Analytical Chemistry;

    分析化学的获奖情况

    • • 1999获首届国家期刊奖
    • • 2000年获中国科学院优秀期刊特别奖
    • • 2001年入选中国期刊方阵“双高”期刊

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