中国葡萄酒中氨基甲酸乙酯的研究
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摘要
氨基甲酸乙酯(Ethyl Carbamate, EC)早在1943年就被证实是一种致癌物质,研究表明,对于啮齿类动物,氨基甲酸乙酯是一种多位点致癌物,可导致肺癌、淋巴癌、肝癌和皮肤癌等疾病,国际癌症研究所把氨基甲酸乙酯对人类的致癌毒性归为2B群。包括葡萄酒在内的发酵饮料和食品中含有微量的氨基甲酸乙酯。加拿大的卫生与预防部门规定佐餐葡萄酒中氨基甲酸乙酯含量不得超过30μg/L;美国食品和药品管理局(US FDA)规定1988年以后生产的佐餐葡萄酒(酒精度≤14%v/v)中氨基甲酸乙酯含量不能超过15μg/L。
论文研究的目的在于建立葡萄酒中氨基甲酸乙酯检测的标准方法,并用该方法对我国葡萄酒中氨基甲酸乙酯的含量进行初步调查,提出我国葡萄酒中氨基甲酸乙酯含量的限量指标建议值,并对葡萄酒中氨基甲酸乙酯的质量控制进行初步探索。
论文主要对以下内容进行了研究:待测葡萄酒样品经预处理后,结合气相色谱-质谱联用的方法对其中氨基甲酸乙酯的含量进行了检测。分别对液/液萃取(Liquid/liquid extraction, LLE)、固相萃取柱萃取(Solid phase extration, SPE)、固相微萃取(Solid phase microextration, SPME)及固/液萃取(Solid/liquid extraction, SLE)四种前处理方法的最佳萃取参数、准确度和精确度进行了研究,并建立葡萄汁中的精氨酸含量的检测方法。通过以上研究,得到如下结果:
液/液萃取法萃取葡萄酒样品中氨基甲酸乙酯时的最佳参数为:酒样溶液的pH为自然pH, KCl用量为16 g (40%),二氯甲烷用量为3×100 mL。方法的检出限为8.0μg/L,回收率在76.56-80.39%之间,相对标准偏差在4.42-9.82%。液/液萃取法用于葡萄酒中氨基甲酸乙酯含量的定量检测,无需贵重仪器,但乳化现象严重,操作系统误差较大,方法的精密度及准确度均较低。
固相微萃取方法萃取的最佳参数为:在搅拌速率800 rpm,溶液平衡30 min的平衡条件下,萃取头选用70μm CW/DVB,NaCl浓度为20-25%,溶液pH10.2,40℃下萃取35 min后,取出萃取头,插入气相色谱-质谱联用的进样口热解析10 min。在此萃取条件下,分析葡萄酒中氨基甲酸乙酯含量的回收率在76.0-84.8%之间,相对标准偏差在6.62-10.95%,检出限8.0μg/L。固相微萃取可以用来检测葡萄酒中氨基甲酸乙酯的含量,方法简便、快速且不需萃取溶剂,是一种环保的样品前处理方法,但方法的精密度和准确度较低。
固相萃取柱方法萃取的最佳pH为样品溶液的自然pH,二氯甲烷的消耗量为175 mL,方法的回收率为85.76-102.82%,相对标准偏差为4.22-8.20%,方法的检出限为3.0μg/L。固/液萃取方法萃取的最佳pH为样品溶液的自然pH,二氯甲烷的消耗量为70 mL,方法的回收率为82.67-93.39%,相对标准偏差为2.91-6.67%,方法的检出限为2.0μg/L。
固/液萃取和固相萃取柱萃取方法准确度高、重现性好,应用这两种萃取方法分析葡萄酒中氨基甲酸乙酯含量没有显著性差异(p<0.05)。国际葡萄与葡萄酒组织(OIV)推荐的方法为固相萃取柱方法,方法中应用的试剂之一无水乙醇本身含有氨基甲酸乙酯,因此存在一定缺陷。同时,和固相萃取柱方法相比,固/液萃取方法萃取成本低,无需贵重仪器和设备,消耗有机溶剂量少,是一种经济、环保、快捷、简便的萃取方法。本研究选择固/液萃取方法为葡萄酒中氨基甲酸乙酯含量检测前处理的标准方法。
用固/液萃取方法对我国61个葡萄酒样品中氨基甲酸乙酯萃取,结合气相色谱-质谱联用分析,结果表明,1997年后生产的葡萄酒中有81.82%的葡萄酒样品中氨基甲酸乙酯含量真实浓度低于15μg/L,参照美国食品和药品管理局、美国葡萄酒研究所和美国酒商协会制定了有关葡萄酒中氨基甲酸乙酯含量的非强制性标准,即1988年以后生产的佐餐葡萄酒(酒精度≤14%v/v)氨基甲酸乙酯含量不能超过15μg/L,因此推荐15μg/L为我国葡萄酒中氨基甲酸乙酯含量限量标准建议值。
通过对氨基甲酸乙酯含量调查结果分析,1996年生产的干红葡萄酒中氨基甲酸乙酯含量最低为未检出,最高含量为28.6μg/L;干白葡萄酒中氨基甲酸乙酯含量最低为未检出,最高含量为13.9μg/L;干红葡萄酒中氨基甲酸乙酯含量高于干白葡萄酒。不同产区之间生产的葡萄酒中氨基甲酸乙酯含量没有显著性差异;贮藏时间对氨基甲酸乙酯的含量有显著性差异,贮藏时间越长,氨基甲酸乙酯含量越高。
对部分原酒样品中氨基甲酸乙酯含量进行潜在浓度的检测,结果表明,氨基甲酸乙酯含量的潜在浓度均超过了加拿大对干红和干白葡萄酒中氨基甲酸乙酯真实浓度规定的限制性标准30μg/L。表明我国还应采取有效措施降低葡萄酒中氨基甲酸乙酯的潜在含量。
葡萄酒中氨基甲酸乙酯的生成与葡萄汁中精氨酸的含量有很大的相关性。葡萄汁中精氨酸在葡萄酒酵母和苹果酸-乳酸菌的代谢下产生氨基甲酸乙酯的前体物质,因此对葡萄汁中精氨酸含量的控制是降低葡萄酒中氨基甲酸乙酯含量的主要途径之一。本研究建立了以离子交换树脂分离提取葡萄汁中精氨酸,然后用坂口试剂检测洗脱液中精氨酸浓度的葡萄汁中精氨酸含量检测的快速方法,方法的最佳检测条件如下。
8-羟基喹啉的次溴酸钠溶液检测葡萄汁中精氨酸含量的最佳条件为:取16 g经预处理的732#离子交换树脂装入玻璃离子色谱柱;将葡萄汁离心,取上清夜,调整其pH为2.0,准确量取待测样品10.0 mL,装入离子交换柱,用蒸馏水淋洗,然后用1 mol/L NaOH洗脱。准确吸取经适当稀释的洗脱液(精氨酸含量大约为1.5-12μg/mL)5.0 mL置于试管中,加入1.0 mL 0.02%的8-羟基喹啉溶液和1.0 mL 10%的NaOH溶液,摇匀,置于冰水浴中,10 min后加入0.5 mL 0.4%的冷次溴酸钠溶液,摇匀,反应1 min,溶液呈铁红色,迅速加入40%尿素1.0 mL,摇匀,用分光光度计进行比色测定,根据标准曲线回归方程计算出葡萄汁中精氨酸含量。
精氨酸浓度在1.5-12μg/mL范围内符合朗姆-比尔定律,摩尔吸光系数为1.45×10~4 L·mol~(-1)·cm~(-1),从葡萄汁的样品分析结果可以看出,相对标准偏差和回收率分别在1.13-2.42%,87.0-100.7%范围内,此方法具有很高的精确度和准确度,适合用于葡萄汁中精氨酸含量的检测。
本研究建立的葡萄酒中氨基甲酸乙酯含量检测的标准方法精密度和准确度较高,并且简便、快捷、环保、经济,适合用于我国葡萄酒中氨基甲酸乙酯含量的检测。建立的葡萄汁中精氨酸含量的快速检测方法适合应用于葡萄种植者和葡萄酒生产厂家用于对葡萄汁中精氨酸含量的适时控制,以便采取措施降低葡萄酒中氨基甲酸乙酯的含量。
Ethyl carbamate, a pluripotent carcinogen, has resulted in an increased incidence of lung, lymphocytic leukemia, liver, and melanotic tumors of the skin, which was first demonstrated in 1943. The International Agency for Research on Cancer (IARC) has classifed ethyl carbamate as a Group 2B, possibly carcinogenic to humans. Most fermented foods and beverages, including wine, contain trace amounts of ethyl carbamate. Health Protection Branch of Canada set the upper limit of 30μg/L ethyl carbamate in table wine; and the U.S. Food and Drug Administration has established a voluntary target for ethyl carbamate of 15μg/L for table wine≤14% alcohol by volume starting with the 1998 harvest.
The purpose of the paper was to develop a simple, accurate and rapid ethyl carbamat analysis standard method for measuring ethyl carbamate in table wine. The developed method could have the application in routine quantification of ethyl carbamate for Chinese table wine. Furthermore, preliminary measures to reduce ethyl carbamate levels in table wine were investigated.
The paper mainly describes the sample-pretreated methods for analyzing ethyl carbamate in table wines in combination with a gas chromatographic/mass spectrometric (GC/MS) system, and n-propyl carbamate used as the internal standard. Parameters were optimized of the sample-pretreated methods including liquid/liquid extraction, solid phase extraction, solid phase microextraction and solid/liquid extraction. Furthermore, the method for determining arginine in grape juice with Sakaguchi reaction following separating arginine with strong cation - exchange resins was developed. The results were as follows:
The parameters of the liquid/liquid extraction method were optimized: the pH of the samples was natural pH, KCl 16 g (40%), dichloromethane 300mL. The limits of detection were 10μg/mL. The recoveries and the precision were 76.56%-80.39% and 4.42-9.82%, respectively. Liquid/liquid extraction method used for determination of ethyl carbamate in table wines dispenses with expensive instruments, however it has drawbacks: severe emulsification; the large amounts of organic solvents used, resulting in a large volume of waste; the low precision and accuracy due to manual concentration steps.
The optimized parameters of the solid phase microextraction of table wine were: sample pH was 10.2, and 9.0 mL sample and 2.0-2.5 g (20-25%) NaCl were added to the vial; the sample vial was shaken for 30min at 40℃at 800 rpm in the agitator for equilibration; A 70μm CW/DVB fiber was inserted into the headspace for 35min at 40℃, then the fiber removed from the sample vial and inserted into the injection port of the GC for 10min. Under this extraction conditions, the recoveries and the presision were 76.00-84.80%, and 6.62-10.95%, respectively. The limits of detection were 8.0μg/mL. The solid phase microextraction technique was successfully applied to determine the ethyl carbamate levels in table wines, and it allows the extraction and concentration to be focused in a single step. The extraction method was rapid and simple, and without the need for any organic solvent, and it was an environmental protecting extraction method. But it has low precision and accuracy due to unstable fibers.
The parameters of the solid phase extraction method were: the pH of the samples was natural pH, dichloromethane 175 mL. The recoveries and the precision were 85.76%-102.82% and 4.22-8.20%, respectivly. The limit of detection was 3.0μg/mL.
And the optimized parameters of the solid/liquid extraction method were: the pH of the samples was natural pH, dichloromethane 70 mL. The recoveries and the precision were 82.67-93.39% and 2.91-6.67%, respectivly. The limits of detection were 2.0μg/mL.
Both solid/liquid extraction and solid phase extraction methods provided good recovery and reproducibility. There was no significant difference between the two methods (p<0.05). Solid phase extraction method was recommended by OIV, but in the OIV method, anhydrous ethanol, one of the reagents, contained ethyl carbamate in itself. Therefore, there was drawback in this method. Furthermore, comparison with the solid phase extraction method, solid/liquid extraction method was less cost, environmental protecting, fast and simple. In the study, the solid/liquid extraction method was selected as the standard method to extract the ethyl carbamate in table wines.
Solid/liquid extraction method in combination with GC/MS was applied to analysis for ethyl carbamate in 61Chinese table wine samples. The results showed that the real contents of ethyl carbamate in 81.82% samples were lower than 15μg/L. According to the U.S. Food and Drug Administration and the U.S. Bureau of Alcohol, Tobacco, and Firearms established voluntary programs, that is, 15μg/L weighted average for table wines≤14% alcohol by volume starting with the 1998 harvest, so 15μg/L was recommended as the maximum limits for ethyl carbamate in Chinese table wine.
According to analysis of investigation of ethyl carbamate levels, the minimum was not detection, whatever in red or white table wine, and the maximum 28.6μg/L in red table wine and 13.9μg/L in white table wine. Obviously, ethyl carbamate levels in red table wines were higher than those in white table wines. There were no significant difference between wine region (p<0.05), and there were significant difference at storage time (p<0.05), namely, the longer storage time, the higher ethyl carbamate levels.
Arginine, one of the most abundant amino acids in grape juice, is closely related to the levels of ethyl carbamate in wines. Arginine is degraded to urea and citrulline, precursors of ethyl carbamate in wine, by the yeast and malolactic bacteria, respectively. Therefore, control of arginine levels in grape juice is one of the most important steps for winemakers to reduce ethyl carbamate in wine. A simple, accurate and rapid arginine separation method by use of 732# ion exchange resins in combination with Sakaguchi reaction for measuring arginine in grape juice was developed. The results were as follows:
Sixteen grams of 732#pretreated ion exchange resins was packed in chromatographic column. Natural grape juice was centrifuged and the upper (10.0 mL, pH 2.0) was loaded to the column, then rinsed with the distilled water, finally, it was eluted with 1mol/L NaOH solution. To a tube containing 5 mL eluate sample (1.5 -12μg/mL arginine), 1.0 mL 0.02% 8-hydroxyquinoline and 1.0 mL 10% NaOH were added sequentially, the solution was mixed thoroughly in the ice bath, after 10min, 0.5 mL 0.4% sodium hypobromite was added rapidly to develop the color. After mixing, 1.0 mL 40% urea was added within 30 seconds, and then its absorbance was read at 500 nm. According to the standard curve and dilution rate, arginine concentration was determined.
The Lambert-Beer law was followed up to an arginine concentration from1.5 to 12μg/mL, and apparent molar absorptivity of the method was 1.45×10~4 L·mol~(-1)·cm~(-1), its recoveries and precison of grape juice samples were 87.0-100.7% and 1.13-2.42% respectivly. The method presented in this paper is accurate and reliable, and it is suitable for determination of L-arginine in grape juice.
The developed standard method of determination of ethyl carbamate in table wines was simple, fast, reproducible and accurate, and the method could be applicable for routine determination of ethyl carbamate in table wines. The method of determination of arginine in grape juice could be applied for grape growers and winemakers to take necessary measure for controlling the level of ethyl carbamate in wine.
论文研究的目的在于建立葡萄酒中氨基甲酸乙酯检测的标准方法,并用该方法对我国葡萄酒中氨基甲酸乙酯的含量进行初步调查,提出我国葡萄酒中氨基甲酸乙酯含量的限量指标建议值,并对葡萄酒中氨基甲酸乙酯的质量控制进行初步探索。
论文主要对以下内容进行了研究:待测葡萄酒样品经预处理后,结合气相色谱-质谱联用的方法对其中氨基甲酸乙酯的含量进行了检测。分别对液/液萃取(Liquid/liquid extraction, LLE)、固相萃取柱萃取(Solid phase extration, SPE)、固相微萃取(Solid phase microextration, SPME)及固/液萃取(Solid/liquid extraction, SLE)四种前处理方法的最佳萃取参数、准确度和精确度进行了研究,并建立葡萄汁中的精氨酸含量的检测方法。通过以上研究,得到如下结果:
液/液萃取法萃取葡萄酒样品中氨基甲酸乙酯时的最佳参数为:酒样溶液的pH为自然pH, KCl用量为16 g (40%),二氯甲烷用量为3×100 mL。方法的检出限为8.0μg/L,回收率在76.56-80.39%之间,相对标准偏差在4.42-9.82%。液/液萃取法用于葡萄酒中氨基甲酸乙酯含量的定量检测,无需贵重仪器,但乳化现象严重,操作系统误差较大,方法的精密度及准确度均较低。
固相微萃取方法萃取的最佳参数为:在搅拌速率800 rpm,溶液平衡30 min的平衡条件下,萃取头选用70μm CW/DVB,NaCl浓度为20-25%,溶液pH10.2,40℃下萃取35 min后,取出萃取头,插入气相色谱-质谱联用的进样口热解析10 min。在此萃取条件下,分析葡萄酒中氨基甲酸乙酯含量的回收率在76.0-84.8%之间,相对标准偏差在6.62-10.95%,检出限8.0μg/L。固相微萃取可以用来检测葡萄酒中氨基甲酸乙酯的含量,方法简便、快速且不需萃取溶剂,是一种环保的样品前处理方法,但方法的精密度和准确度较低。
固相萃取柱方法萃取的最佳pH为样品溶液的自然pH,二氯甲烷的消耗量为175 mL,方法的回收率为85.76-102.82%,相对标准偏差为4.22-8.20%,方法的检出限为3.0μg/L。固/液萃取方法萃取的最佳pH为样品溶液的自然pH,二氯甲烷的消耗量为70 mL,方法的回收率为82.67-93.39%,相对标准偏差为2.91-6.67%,方法的检出限为2.0μg/L。
固/液萃取和固相萃取柱萃取方法准确度高、重现性好,应用这两种萃取方法分析葡萄酒中氨基甲酸乙酯含量没有显著性差异(p<0.05)。国际葡萄与葡萄酒组织(OIV)推荐的方法为固相萃取柱方法,方法中应用的试剂之一无水乙醇本身含有氨基甲酸乙酯,因此存在一定缺陷。同时,和固相萃取柱方法相比,固/液萃取方法萃取成本低,无需贵重仪器和设备,消耗有机溶剂量少,是一种经济、环保、快捷、简便的萃取方法。本研究选择固/液萃取方法为葡萄酒中氨基甲酸乙酯含量检测前处理的标准方法。
用固/液萃取方法对我国61个葡萄酒样品中氨基甲酸乙酯萃取,结合气相色谱-质谱联用分析,结果表明,1997年后生产的葡萄酒中有81.82%的葡萄酒样品中氨基甲酸乙酯含量真实浓度低于15μg/L,参照美国食品和药品管理局、美国葡萄酒研究所和美国酒商协会制定了有关葡萄酒中氨基甲酸乙酯含量的非强制性标准,即1988年以后生产的佐餐葡萄酒(酒精度≤14%v/v)氨基甲酸乙酯含量不能超过15μg/L,因此推荐15μg/L为我国葡萄酒中氨基甲酸乙酯含量限量标准建议值。
通过对氨基甲酸乙酯含量调查结果分析,1996年生产的干红葡萄酒中氨基甲酸乙酯含量最低为未检出,最高含量为28.6μg/L;干白葡萄酒中氨基甲酸乙酯含量最低为未检出,最高含量为13.9μg/L;干红葡萄酒中氨基甲酸乙酯含量高于干白葡萄酒。不同产区之间生产的葡萄酒中氨基甲酸乙酯含量没有显著性差异;贮藏时间对氨基甲酸乙酯的含量有显著性差异,贮藏时间越长,氨基甲酸乙酯含量越高。
对部分原酒样品中氨基甲酸乙酯含量进行潜在浓度的检测,结果表明,氨基甲酸乙酯含量的潜在浓度均超过了加拿大对干红和干白葡萄酒中氨基甲酸乙酯真实浓度规定的限制性标准30μg/L。表明我国还应采取有效措施降低葡萄酒中氨基甲酸乙酯的潜在含量。
葡萄酒中氨基甲酸乙酯的生成与葡萄汁中精氨酸的含量有很大的相关性。葡萄汁中精氨酸在葡萄酒酵母和苹果酸-乳酸菌的代谢下产生氨基甲酸乙酯的前体物质,因此对葡萄汁中精氨酸含量的控制是降低葡萄酒中氨基甲酸乙酯含量的主要途径之一。本研究建立了以离子交换树脂分离提取葡萄汁中精氨酸,然后用坂口试剂检测洗脱液中精氨酸浓度的葡萄汁中精氨酸含量检测的快速方法,方法的最佳检测条件如下。
8-羟基喹啉的次溴酸钠溶液检测葡萄汁中精氨酸含量的最佳条件为:取16 g经预处理的732#离子交换树脂装入玻璃离子色谱柱;将葡萄汁离心,取上清夜,调整其pH为2.0,准确量取待测样品10.0 mL,装入离子交换柱,用蒸馏水淋洗,然后用1 mol/L NaOH洗脱。准确吸取经适当稀释的洗脱液(精氨酸含量大约为1.5-12μg/mL)5.0 mL置于试管中,加入1.0 mL 0.02%的8-羟基喹啉溶液和1.0 mL 10%的NaOH溶液,摇匀,置于冰水浴中,10 min后加入0.5 mL 0.4%的冷次溴酸钠溶液,摇匀,反应1 min,溶液呈铁红色,迅速加入40%尿素1.0 mL,摇匀,用分光光度计进行比色测定,根据标准曲线回归方程计算出葡萄汁中精氨酸含量。
精氨酸浓度在1.5-12μg/mL范围内符合朗姆-比尔定律,摩尔吸光系数为1.45×10~4 L·mol~(-1)·cm~(-1),从葡萄汁的样品分析结果可以看出,相对标准偏差和回收率分别在1.13-2.42%,87.0-100.7%范围内,此方法具有很高的精确度和准确度,适合用于葡萄汁中精氨酸含量的检测。
本研究建立的葡萄酒中氨基甲酸乙酯含量检测的标准方法精密度和准确度较高,并且简便、快捷、环保、经济,适合用于我国葡萄酒中氨基甲酸乙酯含量的检测。建立的葡萄汁中精氨酸含量的快速检测方法适合应用于葡萄种植者和葡萄酒生产厂家用于对葡萄汁中精氨酸含量的适时控制,以便采取措施降低葡萄酒中氨基甲酸乙酯的含量。
Ethyl carbamate, a pluripotent carcinogen, has resulted in an increased incidence of lung, lymphocytic leukemia, liver, and melanotic tumors of the skin, which was first demonstrated in 1943. The International Agency for Research on Cancer (IARC) has classifed ethyl carbamate as a Group 2B, possibly carcinogenic to humans. Most fermented foods and beverages, including wine, contain trace amounts of ethyl carbamate. Health Protection Branch of Canada set the upper limit of 30μg/L ethyl carbamate in table wine; and the U.S. Food and Drug Administration has established a voluntary target for ethyl carbamate of 15μg/L for table wine≤14% alcohol by volume starting with the 1998 harvest.
The purpose of the paper was to develop a simple, accurate and rapid ethyl carbamat analysis standard method for measuring ethyl carbamate in table wine. The developed method could have the application in routine quantification of ethyl carbamate for Chinese table wine. Furthermore, preliminary measures to reduce ethyl carbamate levels in table wine were investigated.
The paper mainly describes the sample-pretreated methods for analyzing ethyl carbamate in table wines in combination with a gas chromatographic/mass spectrometric (GC/MS) system, and n-propyl carbamate used as the internal standard. Parameters were optimized of the sample-pretreated methods including liquid/liquid extraction, solid phase extraction, solid phase microextraction and solid/liquid extraction. Furthermore, the method for determining arginine in grape juice with Sakaguchi reaction following separating arginine with strong cation - exchange resins was developed. The results were as follows:
The parameters of the liquid/liquid extraction method were optimized: the pH of the samples was natural pH, KCl 16 g (40%), dichloromethane 300mL. The limits of detection were 10μg/mL. The recoveries and the precision were 76.56%-80.39% and 4.42-9.82%, respectively. Liquid/liquid extraction method used for determination of ethyl carbamate in table wines dispenses with expensive instruments, however it has drawbacks: severe emulsification; the large amounts of organic solvents used, resulting in a large volume of waste; the low precision and accuracy due to manual concentration steps.
The optimized parameters of the solid phase microextraction of table wine were: sample pH was 10.2, and 9.0 mL sample and 2.0-2.5 g (20-25%) NaCl were added to the vial; the sample vial was shaken for 30min at 40℃at 800 rpm in the agitator for equilibration; A 70μm CW/DVB fiber was inserted into the headspace for 35min at 40℃, then the fiber removed from the sample vial and inserted into the injection port of the GC for 10min. Under this extraction conditions, the recoveries and the presision were 76.00-84.80%, and 6.62-10.95%, respectively. The limits of detection were 8.0μg/mL. The solid phase microextraction technique was successfully applied to determine the ethyl carbamate levels in table wines, and it allows the extraction and concentration to be focused in a single step. The extraction method was rapid and simple, and without the need for any organic solvent, and it was an environmental protecting extraction method. But it has low precision and accuracy due to unstable fibers.
The parameters of the solid phase extraction method were: the pH of the samples was natural pH, dichloromethane 175 mL. The recoveries and the precision were 85.76%-102.82% and 4.22-8.20%, respectivly. The limit of detection was 3.0μg/mL.
And the optimized parameters of the solid/liquid extraction method were: the pH of the samples was natural pH, dichloromethane 70 mL. The recoveries and the precision were 82.67-93.39% and 2.91-6.67%, respectivly. The limits of detection were 2.0μg/mL.
Both solid/liquid extraction and solid phase extraction methods provided good recovery and reproducibility. There was no significant difference between the two methods (p<0.05). Solid phase extraction method was recommended by OIV, but in the OIV method, anhydrous ethanol, one of the reagents, contained ethyl carbamate in itself. Therefore, there was drawback in this method. Furthermore, comparison with the solid phase extraction method, solid/liquid extraction method was less cost, environmental protecting, fast and simple. In the study, the solid/liquid extraction method was selected as the standard method to extract the ethyl carbamate in table wines.
Solid/liquid extraction method in combination with GC/MS was applied to analysis for ethyl carbamate in 61Chinese table wine samples. The results showed that the real contents of ethyl carbamate in 81.82% samples were lower than 15μg/L. According to the U.S. Food and Drug Administration and the U.S. Bureau of Alcohol, Tobacco, and Firearms established voluntary programs, that is, 15μg/L weighted average for table wines≤14% alcohol by volume starting with the 1998 harvest, so 15μg/L was recommended as the maximum limits for ethyl carbamate in Chinese table wine.
According to analysis of investigation of ethyl carbamate levels, the minimum was not detection, whatever in red or white table wine, and the maximum 28.6μg/L in red table wine and 13.9μg/L in white table wine. Obviously, ethyl carbamate levels in red table wines were higher than those in white table wines. There were no significant difference between wine region (p<0.05), and there were significant difference at storage time (p<0.05), namely, the longer storage time, the higher ethyl carbamate levels.
Arginine, one of the most abundant amino acids in grape juice, is closely related to the levels of ethyl carbamate in wines. Arginine is degraded to urea and citrulline, precursors of ethyl carbamate in wine, by the yeast and malolactic bacteria, respectively. Therefore, control of arginine levels in grape juice is one of the most important steps for winemakers to reduce ethyl carbamate in wine. A simple, accurate and rapid arginine separation method by use of 732# ion exchange resins in combination with Sakaguchi reaction for measuring arginine in grape juice was developed. The results were as follows:
Sixteen grams of 732#pretreated ion exchange resins was packed in chromatographic column. Natural grape juice was centrifuged and the upper (10.0 mL, pH 2.0) was loaded to the column, then rinsed with the distilled water, finally, it was eluted with 1mol/L NaOH solution. To a tube containing 5 mL eluate sample (1.5 -12μg/mL arginine), 1.0 mL 0.02% 8-hydroxyquinoline and 1.0 mL 10% NaOH were added sequentially, the solution was mixed thoroughly in the ice bath, after 10min, 0.5 mL 0.4% sodium hypobromite was added rapidly to develop the color. After mixing, 1.0 mL 40% urea was added within 30 seconds, and then its absorbance was read at 500 nm. According to the standard curve and dilution rate, arginine concentration was determined.
The Lambert-Beer law was followed up to an arginine concentration from1.5 to 12μg/mL, and apparent molar absorptivity of the method was 1.45×10~4 L·mol~(-1)·cm~(-1), its recoveries and precison of grape juice samples were 87.0-100.7% and 1.13-2.42% respectivly. The method presented in this paper is accurate and reliable, and it is suitable for determination of L-arginine in grape juice.
The developed standard method of determination of ethyl carbamate in table wines was simple, fast, reproducible and accurate, and the method could be applicable for routine determination of ethyl carbamate in table wines. The method of determination of arginine in grape juice could be applied for grape growers and winemakers to take necessary measure for controlling the level of ethyl carbamate in wine.
引文
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