CN104483430A - Ethoxyamine hydrochloride applied to formaldehyde content determination and testing method of ethoxyamine hydrochloride - Google Patents
Ethoxyamine hydrochloride applied to formaldehyde content determination and testing method of ethoxyamine hydrochloride Download PDFInfo
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 156
- NUXCOKIYARRTDC-UHFFFAOYSA-N o-ethylhydroxylamine;hydron;chloride Chemical compound Cl.CCON NUXCOKIYARRTDC-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000012360 testing method Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- -1 amine hydrochloride Chemical class 0.000 claims description 15
- 238000004458 analytical method Methods 0.000 claims description 14
- 239000012086 standard solution Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000010829 isocratic elution Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000008055 phosphate buffer solution Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000007853 buffer solution Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 3
- 150000001412 amines Chemical class 0.000 claims 1
- 150000003840 hydrochlorides Chemical class 0.000 claims 1
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000001212 derivatisation Methods 0.000 abstract description 2
- 238000004811 liquid chromatography Methods 0.000 description 9
- 235000013405 beer Nutrition 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- LWZHQJFIHKRLKK-UHFFFAOYSA-N ethyl n-hydroxymethanimidate Chemical compound CCOC=NO LWZHQJFIHKRLKK-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000012085 test solution Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000001256 steam distillation Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N acetonitrile Substances CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种应用于甲醛含量检测的乙氧基胺盐酸盐及其测定方法，涉及甲醛含量测定领域。针对现有利用2，4-二硝基苯肼作为衍生剂测定甲醛含量存在的不足，提供了一种样品前处理简单、检出限低、选择性好、灵敏度高的检测甲醛的新衍生方法。所述方法利用乙氧基胺盐酸盐作为衍生剂，采用高效液相色谱法检测甲醛的含量。该方法的衍生产物在流动相中的溶解度大，因此，不需经过萃取这一步骤，为检测甲醛提供了重要的技术支持。
The invention discloses ethoxylamine hydrochloride and a determination method thereof for formaldehyde content detection, and relates to the field of formaldehyde content determination. Aiming at the shortcomings of the existing determination of formaldehyde content using 2,4-dinitrophenylhydrazine as a derivatizing agent, a new derivatization method for detecting formaldehyde with simple sample pretreatment, low detection limit, good selectivity and high sensitivity is provided. . The method utilizes ethoxyamine hydrochloride as a derivatizing agent, and high-performance liquid chromatography is used to detect the content of formaldehyde. The derivative product of this method has high solubility in the mobile phase, so it does not need to go through the extraction step, which provides important technical support for the detection of formaldehyde.
Description
技术领域 technical field
本发明涉及甲醛含量测定领域。 The invention relates to the field of measuring formaldehyde content.
背景技术 Background technique
目前，对于复杂样品的分析，高效液相色谱法是一种最普遍最有效的分析方法之一。高效液相色谱法随着科技水平和仪器水平的高速发展高效液相色谱仪已在分析领域达到普及的程度。而且高效液相色谱具有分析速度快、应用广泛、高灵敏度等优点。因此，对于甲醛含量比较低的样品中使用高效液相色谱法测定也是一种重要的方法。但是，由于甲醛没有内在的发色团以及荧光体，因此，很难用于复杂样品中甲醛的直接测定。一般来说，分析样品中甲醛的含量时，大部分分析方法都需要进行衍生。 At present, for the analysis of complex samples, high performance liquid chromatography is one of the most common and effective analytical methods. High Performance Liquid Chromatography With the rapid development of technology and instrumentation, high performance liquid chromatography has become popular in the field of analysis. Moreover, high performance liquid chromatography has the advantages of fast analysis speed, wide application and high sensitivity. Therefore, it is also an important method to use high performance liquid chromatography for the determination of samples with relatively low formaldehyde content. However, since formaldehyde has no intrinsic chromophore and phosphor, it is difficult to be used for the direct determination of formaldehyde in complex samples. In general, when analyzing the content of formaldehyde in a sample, most analytical methods require derivatization.
现有检测甲醛使用最广泛的衍生剂就是2，4-二硝基苯肼（DNPH），其原理为，甲醛在酸性条件下与2,4-二硝基苯肼在60℃水浴衍生成2,4-二硝基苯腙，经有机溶剂进行萃取，通过一系列处理过程，最后进行高效液相色谱测定。DNPH柱前高效液相色谱法衍生甲醛的检出限很低，但是要保证完全反应需要的时间比较长、反应温度比较高、以及生成的衍生产物在流动相中的溶解度比较小，因此前处理过程比较繁琐。再有就是DNPH在紫外区有吸收，会在液相色谱中出现拖尾现象，对产物峰有一定的影响。 The most widely used derivatizer for detecting formaldehyde is 2,4-dinitrophenylhydrazine (DNPH). The principle is that formaldehyde is derivatized into 2 , 4-Dinitrophenylhydrazone, extracted by organic solvent, through a series of treatment processes, and finally determined by high performance liquid chromatography. The detection limit of formaldehyde derived from DNPH pre-column high-performance liquid chromatography is very low, but it takes a long time to ensure complete reaction, the reaction temperature is relatively high, and the solubility of the generated derivative products in the mobile phase is relatively small, so pretreatment The process is more cumbersome. Another thing is that DNPH has absorption in the ultraviolet region, which will cause tailing phenomenon in liquid chromatography, which will have a certain impact on the product peak.
发明内容 Contents of the invention
本发明的目的是针对以上检测方法的不足，提供一种样品前处理过程简单、检测时间短、选择性好、灵敏度高的检测甲醛含量检测方法。 The purpose of the present invention is to provide a method for detecting formaldehyde content with simple sample pretreatment process, short detection time, good selectivity and high sensitivity for the deficiencies of the above detection methods.
本发明提供一种应用于甲醛含量检测的乙氧基胺盐酸盐。 The invention provides an ethoxylated amine hydrochloride used in the detection of formaldehyde content.
采用高效液相色谱法测定甲醛含量，乙氧基胺盐酸盐作为衍生剂。 The formaldehyde content was determined by high performance liquid chromatography, and ethoxylated amine hydrochloride was used as a derivatizing agent.
本发明还提供一种利用权利要求1所述乙氧基胺盐酸盐检测甲醛含量的测定方法，包括： The present invention also provides a method for determining formaldehyde content using ethoxylated amine hydrochloride according to claim 1, comprising:
①将不同浓度的甲醛标准液分别与乙氧基胺盐酸盐衍生剂混合，然后在205nm波长下进行高效液相色谱分析，通过等度洗脱，根据色谱图中出现的峰面积与甲醛含量作图，绘制标准曲线； ①Mix different concentrations of formaldehyde standard solutions with ethoxyamine hydrochloride derivatives respectively, and then carry out high-performance liquid chromatography analysis at a wavelength of 205nm, through isocratic elution, according to the peak area and formaldehyde content in the chromatogram Graphing, drawing a standard curve;
②将待测液与乙氧基胺盐酸盐衍生剂混合，然后在205nm波长下进行高效液相色谱分析，通过等度洗脱，根据色谱图中出现的峰面积带入标准曲线，得出待测液甲醛浓度。 ② Mix the liquid to be tested with the ethoxylated amine hydrochloride derivatizer, then carry out high-performance liquid chromatography analysis at a wavelength of 205nm, through isocratic elution, and bring into the standard curve according to the peak area appearing in the chromatogram, and obtain The concentration of formaldehyde in the liquid to be tested.
所述①中甲醛标准液与乙氧基胺盐酸盐衍生剂的混合和②中待测液与乙氧基胺盐酸盐衍生剂混合，混合时间均至少20min。 The mixing time of the formaldehyde standard solution and the ethoxylated amine hydrochloride derivative in ① and the mixing of the test solution and the ethoxylated amine hydrochloride derivative in ② are at least 20 minutes.
所述①中甲醛标准液浓度在0～150.0mg·L-1范围之内。 The concentration of formaldehyde standard solution in ① is in the range of 0-150.0 mg·L −1 .
所述乙氧基胺盐酸盐衍生剂溶液可以通过如下方法配制，称取乙氧基胺盐酸盐于pH值为中性或弱酸性的磷酸盐缓冲溶液中，用缓冲溶液定容，得到乙氧基胺盐酸盐衍生剂溶液。 The ethoxylated amine hydrochloride derivative solution can be prepared by the following method, weighing the ethoxylated amine hydrochloride in a neutral or slightly acidic phosphate buffer solution with a pH value, and distilling to volume with the buffer solution to obtain Ethoxylated amine hydrochloride derivatizer solution.
进行液相色谱分析时，色谱柱可为现有进行液相色谱分析时的色谱柱。 When performing liquid chromatography analysis, the chromatographic column can be an existing chromatographic column when performing liquid chromatographic analysis.
所述待测液制备方法与现有公知的测定甲醛含量的样品处理方法相同，可通过水蒸气蒸馏法、超声提取法、水浸泡提取法或超声-三氯乙酸法等得到待测液。 The preparation method of the test solution is the same as the existing well-known sample processing method for determining the formaldehyde content, and the test solution can be obtained by steam distillation, ultrasonic extraction, water immersion extraction or ultrasonic-trichloroacetic acid method.
本发明具有如下有益效果： The present invention has following beneficial effect:
该方法不需要经过萃取，反应温和，且该方法检出限为0.02mg·L-1，相对标准偏差低，为1.1～5.5%，加标回收率为88.0%～108.0%，可以作为一种新的甲醛检测方法。 The method does not need extraction, the reaction is mild, and the detection limit of the method is 0.02 mg·L -1 , the relative standard deviation is low, 1.1-5.5%, and the recovery rate of standard addition is 88.0%-108.0%, which can be used as a New formaldehyde detection method.
附图说明 Description of drawings
图1为本发明甲醛与乙氧基胺盐酸盐反应生成的乙氧基甲醛肟的紫外色谱图； Fig. 1 is the ultraviolet chromatogram of the ethoxy formaldehyde oxime that formaldehyde of the present invention reacts with ethoxy amine hydrochloride to generate;
图2为本发明甲醛标准液的高效液相色谱图； Fig. 2 is the high performance liquid phase chromatogram of formaldehyde standard solution of the present invention;
图3为本发明实施例中啤酒A的高效液相色谱图； Fig. 3 is the high performance liquid chromatogram of beer A in the embodiment of the present invention;
图4为本发明实施例中啤酒B的高效液相色谱图。 Fig. 4 is the high performance liquid phase chromatogram of beer B in the embodiment of the present invention.
具体实施方式 Detailed ways
下面结合具体实施例对本发明做进一步说明。 The present invention will be further described below in conjunction with specific embodiments.
本发明依据原理为：甲醛与乙氧基胺盐酸盐在中性或弱酸性条件下会反应生成稳定的产物乙氧基甲醛肟，反应方程式如下，生成中间产物，反应最终生成反应式右边产物乙氧基甲醛肟： The present invention is based on the principle that formaldehyde and ethoxyamine hydrochloride will react under neutral or slightly acidic conditions to generate stable product ethoxy formaldehyde oxime, the reaction equation is as follows, an intermediate product is generated, and the reaction finally generates the product on the right Ethoxyformaldoxime:
对乙氧基甲醛肟进行液相色谱分析，在205nm出现峰值，如图1所示。 Carry out liquid chromatography analysis to ethoxy formaldehyde oxime, appear peak at 205nm, as shown in Figure 1.
实施例一：对样品采用高效液相色谱法进行测定，包括以下步骤： Embodiment one: adopt high-performance liquid chromatography to measure sample, comprise the following steps:
（1）制备甲醛标准溶液，绘制标准曲线 (1) Prepare formaldehyde standard solution and draw a standard curve
本实施例中，用碘量法对购买的甲醛进行标定，将其配制成0～150.0mg·L-1的甲醛标准液，准确移取5.0mL甲醛标准溶液加入到5mL、pH=4的乙氧基胺盐酸盐衍生剂中，常温下不断搅拌20min,将混合后溶液进入液相色谱进行分析，其高效液相色谱图如图2所示，通过等度洗脱，根据时间定性，峰面积定量，不同浓度的甲醛标准溶液做三次，取平均值，用峰面积与甲醛含量作图，绘制标准曲线，得到回归方程，回归方程A =29.71C + 38.38，线性关系R2=0.9998，A为峰面积，C为甲醛浓度； In this example, the purchased formaldehyde was calibrated by the iodometric method, and it was formulated into a formaldehyde standard solution of 0-150.0 mg·L -1 , and 5.0 mL of formaldehyde standard solution was accurately pipetted into 5 mL of acetone with pH=4. In the oxyamine hydrochloride derivative agent, stir continuously at room temperature for 20 minutes, and enter the mixed solution into liquid chromatography for analysis. For area quantification, formaldehyde standard solutions of different concentrations were made three times, and the average value was taken, and the peak area was plotted against the formaldehyde content to draw a standard curve to obtain a regression equation. The regression equation A = 29.71C + 38.38, the linear relationship R 2 =0.9998, A Be peak area, C is formaldehyde concentration;
本实施例中乙氧基胺盐酸盐衍生剂溶液配制过程为，称取0.2438g乙氧基胺盐酸盐于pH=4的磷酸盐缓冲溶液中，用缓冲溶液定容于500mL的容量瓶中，得到浓度为5mmol·L-1乙氧基胺盐酸盐衍生剂溶液。 The preparation process of the ethoxyamine hydrochloride derivative solution in this example is as follows: weigh 0.2438g of ethoxyamine hydrochloride in a phosphate buffer solution with pH=4, and use the buffer solution to set the volume in a 500mL volumetric flask , to obtain a concentration of 5mmol L -1 ethoxylated amine hydrochloride derivatizer solution.
（2）制备待测液 (2) Prepare the solution to be tested
待测液制备方法可以选用现有技术中公知的测定甲醛含量的样品处理方法，为举例说明，本实施例选用水蒸气蒸馏法，先用过滤法除去啤酒样品中的二氧化碳，麦汁和发酵液，准确移取50.0mL啤酒样品移入250mL蒸馏瓶中，加入20.0mL 1.4mol·L-1的磷酸溶液,用玻璃棒搅拌均匀，立即进行水蒸气蒸馏，收集馏出液定容。经孔径0.45nm滤膜过滤后做液相色谱分析用。取待测液5mL于10mL的比色管中，再加入5.0mL上述乙氧基胺盐酸盐衍生剂，常温下反应20min，进行液相色谱测定分析； The preparation method of the liquid to be tested can be selected from the sample processing method known in the prior art to measure the formaldehyde content. For illustration, the present embodiment selects the steam distillation method, and first removes carbon dioxide, wort and fermented liquid in the beer sample by filtration. , accurately pipette 50.0mL beer sample into a 250mL retort bottle, add 20.0mL 1.4mol·L -1 phosphoric acid solution, stir evenly with a glass rod, conduct steam distillation immediately, collect distillate to volume. After filtering through a filter membrane with a pore size of 0.45nm, it is used for liquid chromatography analysis. Take 5 mL of the solution to be tested in a 10 mL colorimetric tube, then add 5.0 mL of the above-mentioned ethoxyamine hydrochloride derivative, react at room temperature for 20 min, and perform liquid chromatography analysis;
（3）液相色谱测定 (3) Determination by liquid chromatography
本实施例中液相色谱条件如下，也可选用其它液相色谱柱： In the present embodiment, the liquid chromatography conditions are as follows, and other liquid chromatography columns can also be selected:
色谱柱：Syncronis C18柱，规格为150mm×4.6mm I.D. 5μm； Chromatographic column: Syncronis C18 column, the specification is 150mm×4.6mm I.D. 5μm;
流动相：20.0mmol·L-1磷酸二氢钾缓冲溶液、pH=4.0-乙腈,85: 15v/v； Mobile phase: 20.0mmol L -1 potassium dihydrogen phosphate buffer solution, pH=4.0-acetonitrile, 85: 15v/v;
柱温：30℃； Column temperature: 30°C;
流速为1.0mL·min-1； The flow rate is 1.0mL·min -1 ;
检测波长：205nm； Detection wavelength: 205nm;
进样量：5.0μL。 Injection volume: 5.0 μL.
样品经过色谱测定后，得到色谱图，将色谱图上等度洗脱7.78min处峰面积值带入（1）中线性回归方程，可以得到待测液中甲醛含量。 After the sample is chromatographically determined, a chromatogram is obtained, and the peak area value at the 7.78min isocratic elution on the chromatogram is brought into the linear regression equation in (1), and the formaldehyde content in the test solution can be obtained.
为了说明该方法的可行性，进行甲醛标准溶液精密度测试，其结果如表1所示， In order to illustrate the feasibility of this method, carry out formaldehyde standard solution precision test, its result is as shown in table 1,
表1 甲醛标准溶液精密度实验结果 Table 1 Formaldehyde standard solution precision test results
本实施例中啤酒样品的高效液相色谱图分别如图3和图4，根据给出的峰面积1、2，带入线性回归方程，计算结果如表2所示， The high-efficiency liquid chromatograms of the beer sample in the present embodiment are shown in Fig. 3 and Fig. 4 respectively, according to the peak area 1, 2 that provides, bring into the linear regression equation, the calculation result is as shown in table 2,
表2 啤酒样品的加标回收率实验结果 Table 2 The experimental results of the recovery rate of the beer samples
表1和表2结果显示相对标准偏差1.1～5.5%，加标回收率为88.0%～108.0%。 The results in Table 1 and Table 2 show that the relative standard deviation is 1.1-5.5%, and the recovery rate of standard addition is 88.0%-108.0%.
以上内容是结合具体的实施方式对本发明所做的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明的保护范围。 The above content is a further detailed description of the present invention in combination with specific embodiments, and it cannot be assumed that the specific implementation of the present invention is limited to these descriptions. For those of ordinary skill in the technical field of the present invention, without departing from the concept of the present invention, some simple deduction or replacement can be made, which should be regarded as belonging to the protection scope of the present invention.
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