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CN202351223U - Solid-phase extraction column used for measuring benzo[alpha]pyrene in cigarette smoke - Google Patents

Solid-phase extraction column used for measuring benzo[alpha]pyrene in cigarette smoke Download PDF

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Publication number
CN202351223U
CN202351223U CN2011205147413U CN201120514741U CN202351223U CN 202351223 U CN202351223 U CN 202351223U CN 2011205147413 U CN2011205147413 U CN 2011205147413U CN 201120514741 U CN201120514741 U CN 201120514741U CN 202351223 U CN202351223 U CN 202351223U
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column
phase extraction
cavity
solid
pyrene
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杨光宇
陈永宽
缪明明
陈章玉
张群芳
钟佳
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Yunnan Academy of Tobacco Science
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Abstract

本实用新型属于分析化学设施,具体涉及一种用于卷烟烟气苯并[α]芘分析中的固相萃取柱。本固相萃取柱包括柱腔体和柱帽,在柱腔体内上、中、下位置各设有一筛板,分隔成两格填料腔,一格填料腔中装无水硫酸钠填料,另一格填料腔中装硅胶填料。本实用新型可一次过柱就可达到样品干燥和净化的效果,具有简化样品处理步骤、节约样品处理时间的优点,本固相萃取柱具有结构简单,使用方便且成本低的特点。

Figure 201120514741

The utility model belongs to analytical chemistry facilities, in particular to a solid-phase extraction column used in the analysis of benzo[α]pyrene in cigarette smoke. The solid-phase extraction column includes a column cavity and a column cap. A sieve plate is arranged at the upper, middle and lower positions of the column cavity, which are divided into two packing chambers. One packing chamber is filled with anhydrous sodium sulfate packing, and the other Silica gel packing is installed in the lattice packing cavity. The utility model can achieve the effect of sample drying and purification by passing through the column once, and has the advantages of simplifying sample processing steps and saving sample processing time. The solid phase extraction column has the characteristics of simple structure, convenient use and low cost.

Figure 201120514741

Description

一种用于卷烟烟气苯并[α]芘测定的固相萃取柱A solid-phase extraction column for the determination of benzo[α]pyrene in cigarette smoke

技术领域 technical field

本实用新型属于分析化学设施,具体涉及一种用于卷烟烟气苯并[α]芘分析中的固相萃取柱。 The utility model belongs to analytical chemistry facilities, in particular to a solid-phase extraction column used in the analysis of benzo[α]pyrene in cigarette smoke.

背景技术 Background technique

苯并[α]芘是稠环芳烃中最重要的一种致癌物质;尽管卷烟烟气中苯并[α]芘的量极其微小,但由于其致癌作用明显高于其它稠环芳烃,苯并[α]芘已被我国列为卷烟安全性评价的7种指标之一。目前苯并[α]芘的测定方法有薄层色谱法(TLC)、气相色谱-质谱法 (GC-MS)、高效液相色谱法(HPLC)等。寻找简便、快速的苯并[α]芘测定方法具有一定意义。 Benzo[α]pyrene is the most important carcinogen in fused-ring aromatic hydrocarbons; although the amount of benzo[α]pyrene in cigarette smoke is extremely small, its carcinogenic effect is significantly higher than that of other fused-ring aromatic hydrocarbons. [α]pyrene has been listed as one of the seven indicators for cigarette safety evaluation in my country. At present, the determination methods of benzo[α]pyrene include thin-layer chromatography (TLC), gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography (HPLC), etc. It is meaningful to find a simple and rapid method for the determination of benzo[α]pyrene.

我国烟草行业标准采用GC-MS法测定卷烟烟气中的苯并[α]芘。该方法的操作为:用吸烟机捕集烟气总粒相物,然后用环己烷提取总粒相物中的苯并[α]芘,提取液经无水硫酸钠干燥,用固相萃取柱净化,然后再用GC-MS测定。该方法的处理步骤较多且繁杂,样品的干燥和样品净化需要分别进行,因此处理时间较长。 my country's tobacco industry standard uses GC-MS method to determine benzo[α]pyrene in cigarette smoke. The operation of the method is: use a smoking machine to collect the total particulate matter of the flue gas, then extract the benzo[α]pyrene in the total particulate matter with cyclohexane, dry the extract through anhydrous sodium sulfate, and use solid-phase extraction The column was cleaned up, and then determined by GC-MS. This method has many and complicated processing steps, and sample drying and sample purification need to be carried out separately, so the processing time is longer.

发明内容 Contents of the invention

本实用新型的目的在于针对现有技术的不足,提供了一种固相萃取柱,该固相萃取柱可一次过柱就可达到样品干燥和净化的效果,具有简化样品处理步骤、节约样品处理时间的优点。 The purpose of the utility model is to provide a solid-phase extraction column for the deficiencies of the prior art. The solid-phase extraction column can achieve the effect of sample drying and purification by passing through the column once, and has the advantages of simplifying sample processing steps and saving sample processing. advantage of time.

实现本实用新型上述目的所采取的技术方案是:固相萃取柱包括柱腔体和柱帽,在柱腔体内上、中、下位置各设有一筛板,分隔成两格填料腔,一格填料腔中装无水硫酸钠填料,另一格填料腔中装硅胶填料。 The technical solution adopted to realize the above-mentioned purpose of the utility model is: the solid-phase extraction column includes a column cavity and a column cap, and a sieve plate is respectively arranged at the upper, middle and lower positions in the column cavity, which are separated into two packing chambers, one grid Anhydrous sodium sulfate filler is installed in the filler cavity, and silica gel filler is installed in the other filler cavity.

所述的柱腔体的两端口带螺纹,柱帽为带对应螺纹的旋盖,二者通过螺纹连接并压紧柱腔体中的填料。 The two ports of the column cavity are threaded, and the column cap is a screw cap with corresponding threads, and the two are connected by threads to compress the filler in the column cavity.

所述的柱腔体的内径为 1 cm,长度为2 cm,无水硫酸钠填料在柱腔体中所占的体积为硅胶填料的25%。 The inner diameter of the column cavity is 1 cm, the length is 2 cm, and the volume occupied by the anhydrous sodium sulfate filler in the column cavity is 25% of that of the silica gel filler.

本实用新型的有益效果是:柱腔体用筛板分隔成两格,可装入两种填料,一次过柱就可达到样品干燥和净化的效果,和常规固相萃取柱相比简化了样品处理步骤,节约了样品处理时间;柱腔体和柱帽采用螺纹连接的活动结构,用过后可拆开重新装填使用,可节省费用,降低成本,且固相萃取柱装填非常方便;固相萃取柱材料可由制成FEP材料做成,具有很好的耐热性、耐药品和耐溶剂性,还具有出色的阻渗性,可有效防止固相萃取柱在使用过程中有杂质溶出或老化,提高了本实用新型产品的安全性和检测的稳定性。 The beneficial effects of the utility model are: the column cavity is divided into two grids by a sieve plate, and two kinds of fillers can be loaded, and the effect of sample drying and purification can be achieved by passing through the column once, and the sample is simplified compared with the conventional solid phase extraction column. The processing steps save sample processing time; the column cavity and column cap adopt a movable structure of screw connection, which can be disassembled and refilled after use, which can save costs and reduce costs, and the solid phase extraction column is very convenient to fill; solid phase extraction The column material can be made of FEP material, which has good heat resistance, chemical resistance and solvent resistance, and also has excellent permeability resistance, which can effectively prevent the dissolution or aging of impurities in the solid phase extraction column during use , improving the safety and detection stability of the utility model product.

附图说明 Description of drawings

图1是本实用新型固相萃取柱的结构示意图。 Fig. 1 is the structural representation of the solid phase extraction column of the present invention.

其中,1-柱腔体;2-柱帽;3-筛板;4-无水硫酸钠填料;5-硅胶填料。 Among them, 1-column cavity; 2-column cap; 3-sieve plate; 4-anhydrous sodium sulfate packing; 5-silica gel packing.

具体实施方式 Detailed ways

参见图1,本固相萃取柱的材料全部采用FEP做成,柱的直径为1 cm,长度为2 cm,柱腔体1两端开口处加工有螺纹,柱帽2业加工有对应的螺纹。柱腔体1内上、中、下位置各设有一筛板3,通过筛板分隔成两格,在柱的上端装入无水硫酸钠填料4,压实后装上顶部的筛板3、拧紧柱帽2;然后在柱腔体1的下端口装入硅胶填料5,同样压实,装上下端口的筛板3,拧紧柱帽2,固相萃取柱就装填好。样品萃取时,样品溶液从上端(装填无水硫酸钠的一端)进入,先通过无水硫酸钠层干燥,接着再流过硅胶层净化,样品过柱的流速可为10~25mL/min。过完柱后,洗脱液同样从上端进入进行洗脱,洗脱流速可为5~15mL/min。 See Figure 1, the material of this solid phase extraction column is all made of FEP, the diameter of the column is 1 cm, the length is 2 cm, the openings at both ends of the column cavity 1 are processed with threads, and the column cap 2 is processed with corresponding threads . The upper, middle and lower positions of the column cavity 1 are respectively provided with a sieve plate 3, which is divided into two grids by the sieve plate, and anhydrous sodium sulfate filler 4 is placed on the upper end of the column, and the top sieve plate 3 is installed after compaction. Tighten the column cap 2; then put the silica gel filler 5 into the lower port of the column cavity 1, compact it, install the sieve plates 3 at the upper and lower ports, tighten the column cap 2, and the solid phase extraction column is loaded. When the sample is extracted, the sample solution enters from the upper end (the end filled with anhydrous sodium sulfate), first passes through the anhydrous sodium sulfate layer to dry, and then flows through the silica gel layer for purification. The flow rate of the sample passing through the column can be 10-25mL/min. After passing through the column, the eluent also enters from the upper end for elution, and the elution flow rate can be 5-15mL/min.

Claims (3)

1. one kind is used for the solid-phase extraction column that cigarette smoke benzo [α] pyrene is measured; Comprise post cavity and cap; It is characterized in that: the position, upper, middle and lower respectively is provided with a sieve plate in the post cavity; Be separated into two lattice packing cavities, dress anhydrous sodium sulfate filler is adorned silica filler in another lattice packing cavity in the lattice packing cavity.
2. be used for the solid-phase extraction column that cigarette smoke benzo [α] pyrene is measured by claim 1 is described, it is characterized in that: the two-port of post cavity is threaded, and cap is the spiral cover with corresponding screw thread, the two through be threaded and the hold-down column cavity in filler.
3. by the described solid-phase extraction column that is used for cigarette smoke benzo [α] pyrene mensuration of claim 1, it is characterized in that: the internal diameter of post cavity is 1 cm, and length is 2 cm, and anhydrous sodium sulfate filler shared volume in the post cavity is 25% of a silica filler.
CN2011205147413U 2011-12-12 2011-12-12 Solid-phase extraction column used for measuring benzo[alpha]pyrene in cigarette smoke Expired - Fee Related CN202351223U (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
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CN105510463A (en) * 2015-12-10 2016-04-20 苏州国环环境检测有限公司 Method for rapidly detecting benzopyrene in soil
CN107389815A (en) * 2017-07-12 2017-11-24 云南中烟工业有限责任公司 The method and feed liquid dehydration device of lactic acid and butyric acid in a kind of detection tobacco sauce
US10036574B2 (en) 2013-06-28 2018-07-31 British American Tobacco (Investments) Limited Devices comprising a heat source material and activation chambers for the same
US10542777B2 (en) 2014-06-27 2020-01-28 British American Tobacco (Investments) Limited Apparatus for heating or cooling a material contained therein
CN110917659A (en) * 2019-12-11 2020-03-27 福建师范大学福清分校 A dispersive solid phase extraction device
CN112915589A (en) * 2019-12-06 2021-06-08 中国科学院大连化学物理研究所 Filler filling device of solid-phase extraction column and application thereof
US11064725B2 (en) 2015-08-31 2021-07-20 British American Tobacco (Investments) Limited Material for use with apparatus for heating smokable material
US11241042B2 (en) 2012-09-25 2022-02-08 Nicoventures Trading Limited Heating smokeable material
US11452313B2 (en) 2015-10-30 2022-09-27 Nicoventures Trading Limited Apparatus for heating smokable material
US11659863B2 (en) 2015-08-31 2023-05-30 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
US11672279B2 (en) 2011-09-06 2023-06-13 Nicoventures Trading Limited Heating smokeable material
US11825870B2 (en) 2015-10-30 2023-11-28 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
US11924930B2 (en) 2015-08-31 2024-03-05 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
CN118179090A (en) * 2024-05-15 2024-06-14 成都理工大学 A spliced solid phase extraction column

Cited By (17)

* Cited by examiner, † Cited by third party
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US12041968B2 (en) 2011-09-06 2024-07-23 Nicoventures Trading Limited Heating smokeable material
US11672279B2 (en) 2011-09-06 2023-06-13 Nicoventures Trading Limited Heating smokeable material
US11241042B2 (en) 2012-09-25 2022-02-08 Nicoventures Trading Limited Heating smokeable material
US10036574B2 (en) 2013-06-28 2018-07-31 British American Tobacco (Investments) Limited Devices comprising a heat source material and activation chambers for the same
US10542777B2 (en) 2014-06-27 2020-01-28 British American Tobacco (Investments) Limited Apparatus for heating or cooling a material contained therein
US11659863B2 (en) 2015-08-31 2023-05-30 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
US11924930B2 (en) 2015-08-31 2024-03-05 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
US11064725B2 (en) 2015-08-31 2021-07-20 British American Tobacco (Investments) Limited Material for use with apparatus for heating smokable material
US11452313B2 (en) 2015-10-30 2022-09-27 Nicoventures Trading Limited Apparatus for heating smokable material
US11825870B2 (en) 2015-10-30 2023-11-28 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
US12016393B2 (en) 2015-10-30 2024-06-25 Nicoventures Trading Limited Apparatus for heating smokable material
US12219986B2 (en) 2015-10-30 2025-02-11 Nicoventures Trading Limited Article for use with apparatus for heating smokable material
CN105510463A (en) * 2015-12-10 2016-04-20 苏州国环环境检测有限公司 Method for rapidly detecting benzopyrene in soil
CN107389815A (en) * 2017-07-12 2017-11-24 云南中烟工业有限责任公司 The method and feed liquid dehydration device of lactic acid and butyric acid in a kind of detection tobacco sauce
CN112915589A (en) * 2019-12-06 2021-06-08 中国科学院大连化学物理研究所 Filler filling device of solid-phase extraction column and application thereof
CN110917659A (en) * 2019-12-11 2020-03-27 福建师范大学福清分校 A dispersive solid phase extraction device
CN118179090A (en) * 2024-05-15 2024-06-14 成都理工大学 A spliced solid phase extraction column

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