为了解油炸条件对食品中羧甲基赖氨酸(CML)和羧乙基赖氨酸(CEL)含量的影响,以鸡胸肉为原料,选择在不同的植物油种类、油炸温度、油炸时间、油炸次数和油脂连续加热时间条件下对鸡胸肉进行处理,采用高效液相色谱-质谱联用技术分析油炸鸡胸肉样品中CML和CEL的含量.结果表明:高温油炸会显著增加鸡胸肉中CML和CEL的含量,高油酸葵花籽油和菜籽油油炸鸡胸肉中CML含量较低,分别为218.40、226.40 mg/kg,显著低于其他5种油脂,油脂种类对CEL含量的影响不明显;CML和CEL含量随油炸温度的升高和油炸时间的延长呈不断增加趋势,温度越高,CML和CEL的生成速率越大,在220℃条件下油炸5 min的鸡胸肉中CML和CEL的生成速率分别为140℃条件下油炸鸡胸肉的2.53倍和19.02倍;随油炸次数的增加,CML含量略有下降,CEL含量整体变化不明显;随油脂连续加热时间的延长,油炸鸡胸肉中CML和CEL的含量略有下降,CML和CEL的含量均在初始时间油炸时取得最大值,分别为325.00、51.63 mg/kg.因此,油炸增加了食品中CML和CEL的含量,但可以通过优化油炸条件对其进行调控,在保证食品风味的同时提高食品安全性.

[目的]在降低烟梗木质素含量的同时提高发烟剂的负载量对提升加热卷烟用再造烟叶的品质具有重要意义.[方法]采用不同浓度的发烟剂(丙二醇和甘油)处理烟梗碎末,烘干后采用GC-FID、FTIR、TG、SEM等对样品进行表征,通过Klason法测定反应前后烟梗中的木质素含量.[结果]烟梗中木质素含量降低33％～37％;样品中丙二醇的负载量为0.52％～2.57％,甘油的负载量为24.84％～54.10％;丙二醇的存在可极大地提高反应后烟梗碎末的甘油负载量.[结论]该方法在显著降低烟梗碎末中木质素含量的同时,极大提高了烟梗碎末发烟剂的负载量,为加热卷烟用再造烟叶的品质提升提供了新思路.

针对烟用天然香精香料样品,对YC/T 447-2012中糖的测定方法进行优化,建立了经水萃取后,直接利用HPLC-ELSD仪测定烟用天然香精香料中10种水溶性糖(包括鼠李糖、甜菊糖苷、果糖、山梨醇、甘露糖、半乳糖、葡萄糖、肌醇、蔗糖、麦芽糖)的分析方法.结果表明:①与0.02mol/L NaOH溶液相比,利用水萃取后萃取溶液稳定性更好.②向流动相中添加一定量氨水后,各目标物保留时间更稳定.③ELSD气体流速为2.20 L/min,漂移管温度选择80℃时,各目标物峰面积稳定性更好.④10种水溶性糖的检出限在4.19-12.30 μg/mL之间,加标回收率在80.20％～106.00％之间,方法的日内、日间精密度均较好(日内RSD≤4.05％、日间RSD≤6.25％).⑤采用所建立的分析方法对239种烟用天然香精香料中10种水溶性糖进行普查分析,其中检出率最高的5种糖类化合物为葡萄糖、果糖、蔗糖、麦芽糖、山梨醇.

本文介绍了国内8家实验室研究基于图像处理的烟丝宽度测量方法及ISO 20193:2019的精密度及检测效率.结果表明:(1)基于图像处理的烟丝宽度测量方法得到的精密度与ISO 20193:2019处于同一数量级,重复性标准差(S r)与烟丝宽度的比值小于5％,再现性标准差(S R)与烟丝宽度的比值小于8％;(2)基于图像处理的烟丝宽度测量方法比ISO 20193:2019的检测效率高.

For simultaneous determination of ethylene oxide and propylene oxide in mainstream cigarette smoke, a gas chromatography-mass spectrometry (GC/MS) method combined with cold trapping was developed. Mainstream cigarette smoke was generated under ISO smoking condition and passed through a Cambridge filter pad followed by dry ice cooled impingers containing toluene. The levels of ethylene oxide and propylene oxide in the vapour phase of mainstream cigarette smoke were quantified by GC/MS. The samples of 21 domestic and imported cigarettes with different tar deliveries were analyzed using this method. The results showed that:1) The method displayed a good linearity (R2≥0.999 7). The limits of detection (LOD) for ethylene oxide and propylene oxide were 0.03 μg/cig and 6.8 ng/cig, respectively. The recoveries of ethylene oxide and propylene oxide ranged from 91.0% to 101.5% with the intra-day and inter-day precisions between 2.4% and 6.0%. 2) The levels of ethylene oxide and propylene oxide in the mainstream smoke of 21 cigarette samples were between 1.4-17.8 μg/cig and 158.8-1153.0 ng/cig, respectively. This method is simple, reliable, sensitive and suitable for the determination of ethylene oxide and propylene oxide in mainstream cigarette smoke.

Seven major phenolic compounds,including hydroquinone,resorcinol,catechol,phenol,m+p-cresol and o-cresol,in mainstream cigarette smoke were determined by liquid chromatography with two-dimensional column(2D-LC).The conditions of heart-cutting and two dimensional chromatographic separation for resorcinol,and the stability of 2D-LC system were emphatically investigated.The deliveries of the phenolic compounds in mainstream smoke of twelve cigarette samples were tested with the developed method.The results showed that: 1) Resorcinol could be effectively separated from interfering substances by heart-cutting and 2D-LC.2) The detection accuracy of the other phenolic compounds was not influenced.3) The delivery of resorcinol in mainstream cigarette smoke of the test samples ranged from 0.72 to 2.15 μg/cig.

In order to accurately reveal the pyrolysis process of chlorogenic acid(CGA),the pyrolysates of CGA were analyzed at ten temperature ranges,which were divided on the basis of thermogravimetric curve and pyrolytic characteristics of CGA,by an online gas chromatography/mass spectrometry(GC/MS).The results indicated that: 1) The pyrolysis process of CGA could be divided into at least 6 temperature ranges,at which the weight-loss of CGA were 2.94%,0.61%,8.55%,20.29%,34.32% and 9.43%,respectively.2) The major components produced at the ten temperature ranges were as follows: Only water was observed at 30-120 ℃;no products were detected at 120-190 ℃;water,carbon dioxide and quinide-like compounds were formed at 190-260 ℃;carbon dioxide,phenol,catechol,hydroquinone,water and quinide-like compounds were released at 260-325 ℃;comparing with the products at 260-325 ℃,3-hydroxy benzoic acid,benzoic acid and 4-ethyl catechol were new at 325-400 ℃;27 major pyrolysates were identified at 400-500 ℃,besides primary products,these were secondary products,such as 1,3-cyclopentadienes,furan,alkyl phenols,methyl catechols,benzoic acids,aromatic hydrocarbons and multi-benzene ring compounds;the concentrations of carbon dioxide,water and carbon monoxide were higher,which followed by phenol,catechol and 3-methyl phenol at 500-600 ℃;the main volatile components were water,carbon dioxide and carbon monoxide,and there were also a small quantity of benzene,toluene,phenol and 3-methyl phenol at 600-700 ℃;only water,carbon dioxide and carbon monoxide were observed at 700-800 ℃ and 800-900 ℃.The gradient pyrolysate analysis combining with thermogravimetric analysis could provide more information for investigating the pyrolysis process of CGA.

The deliveries of routine chemical analytes,volatile and semi-volatile components in cellulose acetate(CA) filter cigarette smoke or polypropylene(PP) filter cigarette smoke were determined and compared.The results showed that: 1) the deliveries of total particulate matter,nicotine,tar and CO were similar for both CS;2) the deliveries of most volatile and semi-volatile components of PP filter cigarette were higher than or similar to those of CA filter cigarette,moreover the delivery ratios between PP filter cigarette and CA filter cigarette fluctuated widely;3) the deliveries of furfural,furfuryl alcohol,benzene acetaldehyde,pyridine,acetic acid,phenol,o-cresol and m,p-cresol of PP filter CS were much higher than those of CA filter CS.

By investigating the influences of extraction solvents and application rates,extraction modes,demulsification,salting-out,polarity of chromatic columns and relative analytical conditions on the analytical results,a method for simultaneously determining the residual monomers,such as vinyl acetate and ethyl acetate,in polyvinyl acetate emulsion adhesive for cigarette with GC was developed,using water as a demulsifier,n-hexane as an extraction solvent and ethyl butyrate as an internal standard.The results showed that the recoveries of the method were from 77% to 82% with RSDs of 3% and limits of detection under 0.9 μg/g.The method is suitable for quantitative analysis of vinyl acetate and ethyl acetate in polyvinyl acetate emulsion adhesive for cigarette.

A method for determining the main active compounds,including columbianetin acetate,osthole,columbianadin and columbianetin,in the tincture of Radix angelica Pubescens with HPLC-DAD-MS was established to control the quality of the tincture.The results indicated that the combination of MS and DAD was suitable for qualification of the four compounds,while DAD was suitable for quantification.The RSDs of these compounds were below 2%,the recovery of osthole was 104.7% with the limit of detection of 1.093 μg/mL.

Using Novo435 lipase as catalysis and tert-butanol as medium,four glucose fatty acid esters were directly synthesized from glucose and iso-pentanoic acid,n-hexanoic acid,n-octanoic acid,and lauric acid separately.White powder products were prepared after vacuum distillation and purification.These products were identified qualitatively by HPLC/MS.Results showed that the products were dominated with monoesters,and only a small amount of diesters presented.In addition,pyrolysis products of sugar fatty acid esters were studied by Py/GC/MS,and functions of identified degradation were briefly discussed.The applications of sugar fatty esters in cigarette were evaluated by an expert panel,and the glucose fatty acid esters can improve cigarette flavor with improvedr smoothness and less irritancy.