CN104807917A - Method for measuring contents of fructose and glucose in honey - Google Patents
Method for measuring contents of fructose and glucose in honey Download PDFInfo
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- CN104807917A CN104807917A CN201510242702.5A CN201510242702A CN104807917A CN 104807917 A CN104807917 A CN 104807917A CN 201510242702 A CN201510242702 A CN 201510242702A CN 104807917 A CN104807917 A CN 104807917A
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- acetonitrile
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 title claims abstract description 17
- 239000008103 glucose Substances 0.000 title claims abstract description 17
- 229930091371 Fructose Natural products 0.000 title claims abstract description 16
- 239000005715 Fructose Substances 0.000 title claims abstract description 16
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 title claims abstract description 16
- 235000012907 honey Nutrition 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 12
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 title abstract description 11
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 8
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical group O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract 2
- 238000003556 assay Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- PJVXUVWGSCCGHT-ZPYZYFCMSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;(3s,4r,5r)-1,3,4,5,6-pentahydroxyhexan-2-one Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O.OC[C@@H](O)[C@@H](O)[C@H](O)C(=O)CO PJVXUVWGSCCGHT-ZPYZYFCMSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及检测领域，特别是一种蜂蜜中果糖和葡萄糖含量的测定方法。The invention relates to the field of detection, in particular to a method for determining the content of fructose and glucose in honey.
背景技术Background technique
GB/T18932.22-2003《蜂蜜中果糖、葡萄糖、蔗糖、麦芽糖含量的测定方法》中采用液相色谱法测定蜂蜜中果糖、葡萄糖、蔗糖、麦芽糖含量，该方法测定准确，主峰出峰清晰、各组分能够清楚的分离，作为国标，虽然具有高度的准确性和稳定性，但是依然在测试精度上有提高的可能。GB/T18932.22-2003 "Determination of Fructose, Glucose, Sucrose, and Maltose Content in Honey" uses liquid chromatography to determine the content of fructose, glucose, sucrose, and maltose in honey. The method is accurate and the main peak is clear. Each component can be clearly separated. As a national standard, although it has a high degree of accuracy and stability, it is still possible to improve the test accuracy.
发明内容Contents of the invention
本发明的目的在于提供一种分离效率高、测定准确的蜂蜜中果糖和葡萄糖含量的测定方法。The purpose of the present invention is to provide a method for determining the content of fructose and glucose in honey with high separation efficiency and accurate determination.
本发明的技术方案为：一种蜂蜜中果糖和葡萄糖含量的测定方法，包括以下步骤：The technical scheme of the present invention is: a kind of measuring method of fructose and glucose content in honey, comprises the following steps:
步骤1：样品预处理，取样品5g用30ml水溶解后用乙腈定容至100ml，过滤后备用；Step 1: Sample pretreatment, take 5g of the sample and dissolve it with 30ml of water, then dilute to 100ml with acetonitrile, filter and set aside;
步骤2：采用高效液相色谱法进行分析；Step 2: analyze by high performance liquid chromatography;
高效液相色谱法进行分析的参数设置如下：The parameters for HPLC analysis were set as follows:
流动相：乙腈-水；流速：1ml/min柱温：40℃Mobile phase: acetonitrile-water; flow rate: 1ml/min column temperature: 40°C
色谱柱：Thermo Acclaim混合基质色谱柱，4.6μm×250mm，5μm；所述的流动相中乙腈和水的体积比为60:40～80:20。Chromatographic column: Thermo Acclaim mixed-matrix chromatographic column, 4.6 μm×250 mm, 5 μm; the volume ratio of acetonitrile and water in the mobile phase is 60:40 to 80:20.
在上述的蜂蜜中果糖和葡萄糖含量的测定方法中，所述的步骤2所用的高效液相色谱仪的型号为：hermo U3000高效液相色谱仪。In the assay method of fructose and glucose content in the above-mentioned honey, the model of the high-performance liquid chromatograph used in described step 2 is: hermo U3000 high-performance liquid chromatograph.
在上述的蜂蜜中果糖和葡萄糖含量的测定方法中，所述的流动相采用梯度洗脱，梯度洗脱的参数为：In the assay method of fructose and glucose content in the above-mentioned honey, described mobile phase adopts gradient elution, and the parameter of gradient elution is:
0分钟时流动相中乙腈和水的体积比为60:40；The volume ratio of acetonitrile and water in the mobile phase at 0 minutes was 60:40;
8分钟时流动相中乙腈和水的体积比为65:35；The volume ratio of acetonitrile and water in the mobile phase was 65:35 in 8 minutes;
11分钟时流动相中乙腈和水的体积比为70:30；The volume ratio of acetonitrile and water in the mobile phase was 70:30 at 11 minutes;
11分钟至11.1分钟时乙腈和水的体积比变更为80:20；From 11 minutes to 11.1 minutes, the volume ratio of acetonitrile and water was changed to 80:20;
11.1分钟至30分钟时乙腈和水的体积比恒定不变为80:20；11. From 1 minute to 30 minutes, the volume ratio of acetonitrile and water remained constant at 80:20;
0分钟至8分钟以及8分钟至11分钟期间乙腈和水的体积比以恒定的速度增加。The volume ratio of acetonitrile to water was increased at a constant rate during the period from 0 min to 8 min and from 8 min to 11 min.
本发明的有益效果如下：The beneficial effects of the present invention are as follows:
采用上述方案可以有效的提高果糖和葡萄糖的分析精度。The analysis accuracy of fructose and glucose can be effectively improved by adopting the above scheme.
具体实施方式Detailed ways
下面结合具体实施方式，对本发明的技术方案作进一步的详细说明，但不构成对本发明的任何限制。The technical solutions of the present invention will be further described in detail below in conjunction with specific embodiments, but this does not constitute any limitation to the present invention.
实施例1Example 1
一种蜂蜜中果糖和葡萄糖含量的测定方法，包括以下步骤：A kind of assay method of fructose and glucose content in honey, comprises the following steps:
步骤1：样品预处理，取样品5g用30ml水溶解后用乙腈定容至100ml，过滤后备用；Step 1: Sample pretreatment, take 5g of the sample and dissolve it with 30ml of water, then dilute to 100ml with acetonitrile, filter and set aside;
步骤2：采用高效液相色谱法进行分析；Step 2: analyze by high performance liquid chromatography;
高效液相色谱法进行分析的参数设置如下：The parameters for HPLC analysis were set as follows:
hermo U3000高效液相色谱仪hermo U3000 High Performance Liquid Chromatograph
流动相：乙腈-水(梯度洗脱)；流速：1ml/min柱温：40℃Mobile phase: acetonitrile-water (gradient elution); flow rate: 1ml/min column temperature: 40°C
色谱柱：Thermo Acclaim混合基质色谱柱，4.6μm×250mm，5μm；所述的流动相中乙腈和水的体积比为60:40～80:20。Chromatographic column: Thermo Acclaim mixed-matrix chromatographic column, 4.6 μm×250 mm, 5 μm; the volume ratio of acetonitrile and water in the mobile phase is 60:40 to 80:20.
梯度洗脱的参数为：The parameters of gradient elution are:
0分钟时流动相中乙腈和水的体积比为60:40；The volume ratio of acetonitrile and water in the mobile phase at 0 minutes was 60:40;
8分钟时流动相中乙腈和水的体积比为65:35；The volume ratio of acetonitrile and water in the mobile phase was 65:35 in 8 minutes;
11分钟时流动相中乙腈和水的体积比为70:30；The volume ratio of acetonitrile and water in the mobile phase was 70:30 at 11 minutes;
11分钟至11.1分钟时乙腈和水的体积比变更为80:20；From 11 minutes to 11.1 minutes, the volume ratio of acetonitrile and water was changed to 80:20;
11.1分钟至30分钟时乙腈和水的体积比恒定不变为80:20；11. From 1 minute to 30 minutes, the volume ratio of acetonitrile and water remained constant at 80:20;
0分钟至8分钟以及8分钟至11分钟期间乙腈和水的体积比以恒定的速度增加。The volume ratio of acetonitrile to water was increased at a constant rate during the period from 0 min to 8 min and from 8 min to 11 min.
待测样品的制备Preparation of samples to be tested
采用GB/T18932.22-2003中7.1项提取步骤制备待测样品。The sample to be tested was prepared by the extraction procedure in Item 7.1 of GB/T18932.22-2003.
对比例1Comparative example 1
采用GB/T18932.22-2003中7.2项测定步骤测定。It is determined by the measurement procedure of item 7.2 in GB/T18932.22-2003.
测试结果：Test Results:
实施例1的果糖出峰时间为6.225min，葡萄糖出峰时间为9.357min；The fructose peak time of embodiment 1 is 6.225min, and the glucose peak time is 9.357min;
对比例1的果糖葡萄糖时间为7.851min，葡萄糖出峰时间为9.254min；The fructose glucose time of comparative example 1 is 7.851min, and the glucose peak time is 9.254min;
通过实施例1的方法，出峰分离更加明显，可以提高测试的准确性。By the method of Example 1, the peak separation is more obvious, which can improve the accuracy of the test.
以上所述的仅为本发明的较佳实施例，凡在本发明的精神和原则范围内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and any modifications, equivalent replacements and improvements made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510242702.5A CN104807917A (en) | 2015-05-12 | 2015-05-12 | Method for measuring contents of fructose and glucose in honey |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114088833A (en) * | 2021-11-17 | 2022-02-25 | 广州浩宇生物科技有限公司 | Method for rapidly detecting glucose content in food |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005080515A (en) * | 2003-09-04 | 2005-03-31 | Suntory Ltd | Novel α-glucosidase and process for producing the same |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005080515A (en) * | 2003-09-04 | 2005-03-31 | Suntory Ltd | Novel α-glucosidase and process for producing the same |
Non-Patent Citations (5)
| Title |
|---|
| THERMO FISHER SCIENTIFIC INC: "Sugars in a Sports Beverage Using Acclaim Trinity P2 in HILIC Mode", 《THERMO SCIENTIFIC》 * |
| THERMO FISHER SCIENTIFIC INC: "Sugars in Honey Using Accucore 150-Amide-HILIC", 《THERMO SCIENTIFIC》 * |
| 中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《中华人民共和国国家标准 GB/T 22221-2008》", 16 May 2008 * |
| 国家质量监督检验检疫总局: "《GB/T 18932.22-2003》", 1 January 2003 * |
| 张书芬 等: "液相色谱示差折光法测定蜂蜜中的果糖、葡萄糖、蔗糖和麦芽糖", 《食品科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114088833A (en) * | 2021-11-17 | 2022-02-25 | 广州浩宇生物科技有限公司 | Method for rapidly detecting glucose content in food |
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