CN105158349A - 高温灰化-离子色谱分析茶叶中f-含量 - Google Patents
高温灰化-离子色谱分析茶叶中f-含量 Download PDFInfo
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Abstract
本发明涉及高温灰化-离子色谱系统,特别涉及高温处理茶叶样品,马弗炉中500-550℃高温灰化4-5h,超纯水溶解,经0.45μm滤膜过滤的处理,然后采用离子色谱测定茶叶中的F-。本发明灵敏度高,准确性好。
Description
技术领域
本发明涉及一种高温烘箱和化学仪器分析的使用系统,特别涉及检测茶叶中F-的高温灰化-离子色谱分析系统。
背景技术
中国有民以茶代礼的风俗,茶已经成为世界上除水以外消耗量最大的饮料。茶树鲜叶经过不同的加工处理方式可以制成不同类型的茶叶,有绿茶、红茶、黄茶、黑茶、乌龙茶、白茶等种类。茶作为一种经常饮用的饮料,它含有的F-等阴离子的浓度高低与人体的健康密切相关。近年来,无机阴离子的价值和危害开始受到社会大众越来越多的关注。在日常生活饮水和饮茶的过程中,适当的摄入某些无机阴离子对人体是有益的,但是过量的摄入某些阴离子将会对人体造成潜在的影响。茶叶中的F-是人体内的必需微量元素,摄入适量的F-有利于牙齿健康,防止龋齿发生;但摄入过量的F-对身体有害,易造成斑釉齿症或氟骨症。因此对茶叶中阴离子的含量进行测定,有利于保证茶叶的品质,同时对保护人体的身体健康也具有一定的意义。
目前,测定茶叶中无机阴离子的方法有很多.按照GB/T5009.18-2003中用比色法测定茶叶中的氟离子,其操作繁琐,需要花费较多的人力、时间和试剂等;用毛细管电泳分离间接检测方法测定茶叶中的阴离子,其各种阴离子的检出限的范围为0.11~0.82mg·L-1,相对标准偏差为1.2%~3.8%;以上这几种测定方法的检出限和相对标准偏差都较高,实验方法的灵敏度和准确性都不强。
用水浸提茶叶后,直接采用离子色谱分析,F-的检测结果在3000ppm以上。采用C18小柱预处理小柱对茶叶水,而后采用离子色谱,F-检测结果在600mmp以上。而根据我国农业部的规定,茶叶中F-的含量不能超过200ppm。显然采用C18小柱预处理茶叶水或不处理茶叶水,采用离子色谱分析,测定茶叶中F-的误差较大。而引起这种误差的原因主要是因为C2O4 2-和F-的保留时间接近,C2O4 2-的峰面积与F-的峰面积部分重合。因此,测定结果F-含量偏大。采用高温灰化-离子色谱分析茶叶中F-,结果表明:本法准确可靠,重复性好,干扰少,快速,利于更好检测茶叶中F-,同时,也为检测茶叶中F-提供了新方法。
发明内容
本发明正是针对现有检测技术的不足之处,提供一种高温灰化-离子色谱分析系统用以测定茶叶中的F-含量,该系统简化了茶叶中F-的检测技术,缩短了分析时间,提高了准确性。
本发明通过高温灰化,消除茶叶中有机酸,尤其是C2O4 2-对F-离子的影响,而后直接进行离子色谱分析茶叶中的F-,而不需要其他预处理。
本发明也可应用于花茶中F-含量的分析,同时提高灵敏度和改善检测限。
本发明具有以下优点
本发明采用高温灰化除去茶叶中的有机酸,消除了C2O4 2-对F-的影响。与采用C18柱预处理相比,省去了C18柱的消耗,同时,完全消除了C2O4 2-,提高了准确度。
附图说明
图1为本发明的F-离子色谱图。
具体实施方式:
下面通过具体实施例对本发明的技术方案做进一步说明:
1材料:碧螺春、黄山毛峰、西湖龙井、信阳毛尖茶叶氟化钠、氯化钠、硝酸钾、硫酸钠、碳酸钠水为超纯水。
2实验仪器:离子色谱仪:IC6000型,色谱柱:SI-524E型,自动进样器:AS2800,安徽皖仪科技股份有限公司;
3称取有机纯品氟化钠溶于超纯水中制成混合标准品母液,使混合标准母液中氟离子为200μg·mL-1。然后将母液通过逐级稀释,混合标准溶液的浓度为1#标准液,2ppm;2#标准液,1ppm;3#标准液,0.5ppm;4#标准液,0.1ppm;5#标准液,0.02ppm。混合标准母液最长保留时间不能超过一周。
4离子色谱分析工作条件,SI-524E型阴离子色谱柱,淋洗液为3.6mmol·L-1碳酸钠,流速为0.7mL·min-1,柱温为45℃,池温为40℃,抑制器电流为40mA,满程进样。
5标准曲线的制作。把配制好的标准品溶液,满程进样到离子色谱中。分别记录浓度及色谱中的峰面积。根据浓度和峰面积做出标准曲线。
6将干燥的茶叶样品粉粹,充分磨碎均匀后各取0.5000g,分别放入坩埚内。用电炉低温加热炭化,移入马弗炉中550℃灰化4h,冷却取出。将灰化完全的茶叶样品置于50mL的小烧杯中,加入少量高纯水溶解,使茶叶样品中的阴离子充分溶解,用0.45μm滤膜过滤;将滤液定容至50mL容量瓶中,离子色谱测定。
7加标回收试验,用精密度试验的茶叶样品12个平行样,分别加入氟离子标准品溶液到茶叶中,添加量0.4mg·kg-1。灰化处理后,做离子色谱法的加标回收率试验。结果表明,氟离子在0.02-2μg·mL-1的浓度范围内有良好的线性关系;F-的检出限为0.01ppm。
8茶叶样品中F-的加标回收率为95.0%~104.5%。碧螺春含F-为12.5ppm,黄山毛峰13.0ppm,西湖龙井6.0ppm,信阳毛尖7.0ppm。
Claims (3)
1.高温灰化-离子色谱分析系统,其特征在于,茶叶样品500-550℃高温灰化4-5h。
2.高温灰化-离子色谱分析系统,其特征在于,通过样品高温灰化后,一些易挥发的有机酸分解,而不需要进行其他预处理,超纯水溶解后灰分后,滤膜过滤后,可直接采用离子色谱分析样品中F-的含量。
3.根据权利要求2所述的方法,其特征在于,该方法也可以应用花茶中F-含量的测定。
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CN110057963A (zh) * | 2019-05-24 | 2019-07-26 | 南京江原安迪科正电子研究发展有限公司 | 一种Na18F注射液中氟离子含量的高效液相色谱检测方法 |
CN112083102A (zh) * | 2020-09-15 | 2020-12-15 | 安徽皖维高新材料股份有限公司 | 一种测定pva中硫酸根离子含量的方法 |
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JP2011021928A (ja) * | 2009-07-14 | 2011-02-03 | Fuji Electric Holdings Co Ltd | 金型成形用のハロゲン系難燃剤含有樹脂を選択する方法 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110057963A (zh) * | 2019-05-24 | 2019-07-26 | 南京江原安迪科正电子研究发展有限公司 | 一种Na18F注射液中氟离子含量的高效液相色谱检测方法 |
CN112083102A (zh) * | 2020-09-15 | 2020-12-15 | 安徽皖维高新材料股份有限公司 | 一种测定pva中硫酸根离子含量的方法 |
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