本文研究了一种适用于各类饮用酒酒精度检测的方法.以蒸馏酒、发酵酒、配制酒为研究对象,采用自动蒸馏结合数字密度仪法测定其酒精度,通过与GB 5009.225-2016《食品安全国家标准酒中乙醇浓度的测定》中的密度瓶法、酒精计法比对,探究该方法用于检测各类酒酒精度的适用性.研究表明,自动蒸馏结合数字密度仪法适用于各类饮用酒酒精度的含量检测,具有节约样品、省时、省力、高效的特点,检测结果的精密度、重复性和准确性均符合GB 5009.225-2016《食品安全国家标准酒中乙醇浓度的测定》和GB/T 27404-2008《实验室质量控制规范食品理化检测》的相关要求,适合口岸进出口大批量样品检测.

食品的营养标签通过向消费者直接展示产品特性,引导消费者合理选择食品,标签准确规范才能保证消费者不受误导.本文对预包装食品营养标签标示常见问题进行汇总与分析,提高预包装食品营养标签标示水平,保护消费者合法权益.

目的 建立分散液液微萃取结合气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)测定葡萄酒中20种农药残留的分析方法.方法 样品经水稀释后,采用60μL氯仿和940μL乙腈进行分散液液微萃取,3000 r/min离心5 min,浓缩后采用气相色谱-质谱联用仪检测.结果 在白葡萄酒与红葡萄酒中进行2.5、5.0、10.0μg/L的添加回收实验,本方法的平均回收率为66.7％～126.1％,相对标准偏差为1.3％～27.2％,方法的检出限为0.025～0.690μg/L,定量限为0.082～2.300μg/L.结论 本方法前处理过程简单、快速、灵敏度极高、定量结果准确,适用于葡萄酒中多种农药残留的检测.

以发酵酒、配制酒和蒸馏酒三大酒类为研究对象,采用经济而操作简单的直接酒精计法,与传统的国标方法进行方法比较,研究该方法在各大酒类中的适用性.研究表明,该方法操作简便、经济快速,可实现在白酒、伏特加、朗姆酒、威士忌、龙舌兰酒和金酒这6种蒸馏酒中酒精度的快速测定,与GB 5009.225-2016中规定的第二法相比,测定结果重现性及准确性都符合要求,适用于对这6类蒸馏酒的日常酒精度检测需求.

建立直接测定甜型葡萄酒中高浓度总二氧化硫的微流-连续流动注射分析方法.样品用10％的硫酸酸化,在酸性条件下蒸馏,蒸馏液与甲醛和碱性品红反应生成红色络合物,吸取样品并配制好相应试剂后,采用微流-连续流动分析仪在560 nm波长处自动完成分析.对影响测定的酸化液浓度、碱性品红和甲醛浓度等进行了优化,确定了最佳试验参数.结果显示,二氧化硫标准溶液在25～250 mg/L范围内可呈现良好的线性,线性相关系数大于0.999,检出限为4.6 mg/L,起泡葡萄酒样品加标回收率在92.4％～108.8％范围内,相对标准偏差≤5.3％(n=6).该方法为甜型葡萄酒中高浓度二氧化硫的直接测定提供了一个自动化、高效、准确的快速检测方法.

A method was established for the detection of 10 whitening and 2 prohibited components in cosmetics by high performance liquid chromatography (HPLC).Low fat cosmetics samples such as make-up water and lotion were extracted directly with 0.02 mol/L potassium dihydrogen phosphate solution(pH 6.0).High fat cosmetics samples and wax based and powder cosmetics were well dispersed with 2.5 mL dichloromethane first,then extracted with 0.02 mol/L potassium dihydrogen phosphate solution (pH 6.0).The sample solution were centrifuged at a speed of 9 500 r/min,then filtered through a 0.22 μm syringe filter.The filtrate were analyzed on an Eclipse XDB-C18 column (250 mm ×4.6 mm,i.d 5 μm) using 0.02 mol/L potassium dihydrogen phosphate (pH 6.0)-methanol as mobile phase at a flow rate of 1.0 mL/min.The temperature of the column was set at 25 ℃.The detection wavelengths were 230 nm and 250 nm.The standard working curves of 12 compounds had good linear relationships(r ＞ 0.999 0) in concentration range of 2.5-100 mg/L.The quantitation limits(S/N =10) of 12 compounds wcre in the range of 0.006 5％-0.025％.The recoveries of 12 analytes at spiked levels of 0.025％-0.5％ were in the range of 87％-102％ with relative standard deviations less than 4％.With the advantages of simplicity,high recovery and good precision,this methed was suitable for the determination of 10 whitening and 2 prohibited components in cosmetics.

A method has established for the detection of vitamin C (VC) and its derivatives (ascorbyl glucoside, AA-2G; magnesium ascorbyl phosphate, AA-2P; ascorbic acid ethyl ether, Only VCE) in cosmetics by high performance liquid chromatography (HPLC). Low fat cosmetic samples such as make-up water and lotion were extracted directly with 30 mL 0.02 mol/L potassium dihydrogen phosphate solution (pH 3.0). High fat cosmetic samples such as face cream and gel were well dispersed with 1.0 mL dichloromethane first, then extracted with 25 mL 0.02 mol/L potassium dihydrogen phosphate solution (pH 3.0). The sample solution was centrifuged with a speed of 12,000 r/min, then filtered through a 0.22 μm syringe filter. The filtrate was analyzed on a column of YMC-Triart C18 (250 mm x 4.6 mm, 5 μm) using 0.02 mol/L potassium dihydrogen phosphate solution (pH 3.0) and methanol as mobile phases with a flow rate of 1.0 mL/min. The temperature of the column was 25 °C and the detection wavelength was 250 nm. The standard working curves of the four analytes had good linear relationship (r2>0.9999). The detection limits of the four analytes were 0.04-0.08 g/kg (S/N=10). The recoveries were 95.6%-101.0% with the relative standard deviations of 0.62%-3.0% at the spiked levels of 0.25-5.0 g/kg. This method is a simple, rapid, exact and reliable for the determination of the contents of vitamin C and its derivatives in cosmetics.

目的:建立空气隔断-连续流动分析仪快速测定葡萄酒中总糖含量的分析方法.方法:用样品校正葡萄糖标准溶液,同时在流路中增设透析器以减少样品溶液带来的基质效应及颜色干扰.经过条件优化,流路温度控制在88～92℃,水解反应时间、络合反应时间分别为5min和12 min.结果:在0.05～3.0 g/L质量浓度范围内,体系吸光度与溶液质量浓度线性关系良好(r2为0.9997),方法检出限为0.01 g/L,加标回收率在88.1％～102.3％之间,方法相对标准偏差为2.8％～6.2％;测定结果与GB/T 15038-2006《葡萄酒、果酒通用分析方法》相比,相对标准偏差小于5％,测定快速(45样/h).结论:方法适用于大批量葡萄酒中总糖含量的检测.

目的 了解深圳市市售美白祛斑化妆品中美白祛斑剂及铅、砷、汞的含量,美白祛斑成分与样品标签符合情况,有助于建立美白祛斑产品的卫生安全及功效成分评价体系,以规范市场.方法 对深圳市市售的110份化妆品进行8种美白祛斑剂和铅、砷、汞含量检测.结果 110份样品均未检出禁用美白祛斑剂氢醌、苯酚和曲酸,2份样品检出高浓度的汞,其余样品铅、砷、汞含量均符合《化妆品卫生规范》(2007年版)要求.美白祛斑剂检出率为45.5％,标签符合率为62.2％.结论 深圳市售的化妆品美白祛斑剂含量总体是符合我国《化妆品卫生规范》(2007年版)要求的.美白祛斑功效成分含量偏低,样品存在标签不符情况,提示管理部门应加强产品监督,打击虚假宣传及三无产品.

An analytical method was developed for the simultaneous determination of 25 quinolones, including danofloxacin mesylate, enrofloxacin, flumequine, oxloinic acid, ciprofloxacin, sarafloxacin, nalidixic acid, norfloxacin, and ofloxacin etc in cosmetics using direct extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Cosmetic sample was extracted by acidified acetonitrile, defatted by n-hexane and separated on Poroshell EC-C18 column with gradient elution program using acetonitrile and water (both containing 0. 1% formic acid) as the mobile phases and analyzed by LC-ESI-MS/MS under the positive mode using multiple reaction monitoring (MRM). The interference of matrix was reduced by the matrix-matched calibration standard curve. The method showed good linearities over the range of 1-200 mg/kg for the 25 quinolones with good linear correlation coefficients (r ≥ 0.999). The method detection limit of the 25 quinolones was 1.0 mg/kg, and the recoveries of all analytes in lotion, milky and cream cosmetics matrices ranged from 87.4% to 105% at the spiked levels of 1, 5 and 10 mg/kg with the relative standard deviations (RSD) of 4.54%-19.7% (n = 6). The results indicated that this method is simple, fast and credible, and suitable for the simultaneous determination of the quinolones in the above three types of cosmetics.

Objective To investigate the distribution of typical EDCs in Pearl River estuaries.Methods Sur-face sediment were collected, and EDCs were extracted by accelerated solvent extraction (ASE) from sediment matrix and cleaned up by centrifugation, the target compounds were finally analyzed by GC-MS after derivati-zation by BSTFA.Results Industrial EDCs such as OP, NP, BPA, and PP, steroidal EDCs such as natural es-trogens E1, E2, and synthetical estrogen EE2 were widely detected. Except the detection percent was 88.2% for EE2, the other EDCs were detected in all the collected samples, and the concentration ranges (ng/g dw) were in the following order: NP(565.28~812.6)>BPA(42.55~248.25)>PP (93.44~109.96)>OP (3.62~11.52), E1(14.13~ 23.13), E2(6.86~15.42), and EE2(ND~23.45).Conclusion Spatial distribution of the 4 industrial EDCs and EE2 were similar, concentration in the east four outlets were higher than that in the west four outlets, and espe-cially higher in Humen estuary. Moreover, EDCs concentrations in each estuary decreased gradually with stream direction from river to ocean. Except possible point pollution source in Jitimen, E1 and E2 concentration in the other seven outlets were in the same magnitude.

建立了同时检测糖果中喹啉黄、孟加拉红、坚牢绿、酸性红52、荧光素钠、曙红、酸性绿S、亮黑、荧光桃红等9种禁限用色素的高效液相色谱分析方法.糖果样品经水振荡溶解,离心过滤后用高效液相色谱法测定,外标法定量.9种禁限用色素在0.2～50 mg/L范围内线性良好,加标收率在88.2％～97.3％之间,相对标准偏差(RSD)小于5％.结果表明,该方法简便、快速,准确,灵敏度及精密度高,适用于糖果中9种禁限用色素的测定.

Objective To develop a method to determine residues of 5 milbemycins-moxidectin, milbe-mycin A3, milbemycin A4, milbemycin D and nemadectin in milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS).MethodsThe residues of milbemycins in milk samples were extracted by aceto-nitrile and purified by a C18 SPE column. After being separated by an Agilent Poroshell 120 EC-C18 chromato-graphic column with gradient elution using 0.1% formic acid aqueous and methanol, the extracts were deter-mined by LC-MS/MS under the positive ion mode with multi-reaction monitoring (MRM).ResultsThe cali-bration curves of 5 milbemycins were linear in the range of 10~100 μg/kg, with the correlation coefficients (R) >0.99. Average recoveries were 77.5%~100% with relative standard deviations less than 11.6%. Conclu-sionThe method is suitable for the determination of milbemycins residues in milk due to its high sensitivity and good reproducibility.

为了解决进口葡萄酒来源复杂,原产地难鉴别的问题,使用电感耦合等离子体质谱检测葡萄酒中的元素含量,采用偏最小二乘法建立聚类分类模型用于原产地鉴别.电感耦合等离子体质谱检测了澳大利亚、智利、法国、意大利和西班牙5个国家的100份葡萄酒中的41种元素,通过变量两两相乘进行扩维,偏最小二乘法变量筛选方法对扩维后的大量变量进行处理,删除冗余变量和影响不显著的变量,建立了聚类分析模型,模型可以很好地将各国葡萄酒样品区分,分辨准确率在96％以上.将来自5个国家的99份和南非的11份葡萄酒样品检测数据代入模型,判别结果令人满意.

A discrimination method for 6 kinds of Chine se famous tea by combination of organic components and multielement analysis was established. Totally 67 different tea samples from their places of origin were collected, including green tea(Huangshan Maofeng, West Lake Longjing, Biluochun and Lushan Fragrant) and oolong tea(Wuyi Rock Tea, Ti Kuan Yin). The concentrations of 9 elements(K, Ca, Mg, Al, Mn, Fe, Zn, Rb and Ti) were determined by ICP-AES, 12 elements(Pb, As, Cd, Cr, V, Ni, Co, Cu, Sr, Cs, Ba and Se) by ICP-MS, and 10 organic compounds by UPLC. Partial least squares variable selection method was applied in the establishment of the discrimination models for elements and organic components, and a tracing procedure was set up for the confirmation of the known and unknown tea samples. The analysis of real samples showed that the 6 kinds of Chinese famous tea were well discriminated and misjudgment was reduced effectively by cross validation of the two models.

This article reviews the study progress of the pre-treatment technology and the analytical methods at home and abroad in wine traceability by aroma in recent years. Furthermore, the application of the combination of these techniques and the chemometrics methods in this field has been discussed.

目的 建立超高效液相色谱(UPLC)同时测定茶叶中没食子酸(GA)、茶碱(THEO)、咖啡因(CAFF)、没食子儿茶素(GC)、儿茶素(C)、表儿茶素(EC)、表没食子儿茶素(EGC)、表没食子儿茶素没食子酸酯(EGCG)、没食子儿茶素没食子酸酯(GCG)、表儿茶素没食子酸酯(ECG)的分析方法.方法 以甲醇-水-磷酸为流动相,BEH C18分离,梯度洗脱,230 nm波长检测,结果 10种组分的线性范围为:0.1 mg/L ～ 20 mg/L1,回收率在94.9％～ 102.3％,RSD为0.7％～4.09％.结论 方法简便、重现性好,灵敏度高.

A liquid chromatography-tandam mass spectrometric(LC-MS/MS) method was developed for the simultaneous identification and determination of residues of carbadox(CBX),olaquindox and related metabolites,desoxycarbadox(DCBX),quinoxalie-2-carboxylic acid(QCA) and 3-methylquinoxaline-2-carboxylic acid(MQCA) in bovine and porcine muscle and liver tissues.CBX was extracted by acetonitrile-ethyl acetate(1∶1,by volume).As for the extraction of DCBX,QCA and MQCA,homogenized liver or muscle tissue was first digested with 0.6%formic acid to deactivate naturally-occurring enzymes.After overnight enzymatic hydrolysis with protease,the tissue extract was acidified,centrifuged and filtered.DCBX,QCA and MQCA were recovered from the tissue extract using an Oasis MAX solid phase extraction(SPE) cartridge.The analytes were separated on an Inertsil ODS-3 LC column,and determined qualitatively and quantitatively under multi-reaction monitoring(MRM) scan type with tandem mass analyzer using positive polarity mode.The limits of quatitation(LOQ) for the four analytes in bovine and porcine muscle and liver tissues were 0.5 μg/kg.At the spiked level in the range of 0.5-5.0 μg/kg,the mean recoveries were in the range of 76%-97%,the relative standard deviation were in the range of 2.9%-16.9%.

The aim of this research is to investigate the enzymatic preparation of angiotensin I-converting enzyme inhibitory peptide(ACEIP) on the basis of the structure information analysis and by choosing enzymes with preferential specificity,thus preliminarily giving a directional and controlled enzymolysis technology according to the structure information.In the investigation,the structure information of 11 selected angiotensin I-converting enzyme inhibitors was analyzed by means of the Complete Neglect of Differential Overlap(CNDO).The results indicate that the oligopeptide possesses high inhibitory activity to angiotensin I-converting enzyme(ACE) when it is of residues Pro, Trp,Met,Phe and Lys in C-terminal position and when residues Asp and Glu in N-terminal position.Then,the enzymatic preparation of ACEIP from tilapia meat was conducted using enzymes with preferential specificity.The hydrolysate,in which Thr-Cys,Asp-Trp and Glu-Met were found,was finally extracted and analyzed.The results accord with the theoretical results,which preliminarily shows the feasibility of the directional and controlled enzymatic technology based on the structure information.

The enzymatic hydrolysis of the tilapia offal by different enzymes was studied. According to the content of amino nitrogen(Cn), the content of TCA soluble peptide(Cp)during the enzymatic hydrolyzing as well the flavor of the enzymatic production, the hydrolysate with the better content of amino nitrogen and the flavor were conducted by Flavourzyme Protame, Flavourzyme and Alcalase 2.4L. After improving the hydrolyzing process,the Cn of hydrolysate by the Flavourzyme and Protame, Flavourzyme and Alcalase 2.4L reached 0.4%,0.35% respective.