技术领域technical field
本发明涉及食品安全检测技术领域，具体涉及一种高粱籽粒中含氮化合物含量的测定方法。The invention relates to the technical field of food safety detection, in particular to a method for determining the content of nitrogen-containing compounds in sorghum grains.
背景技术Background technique
随着人们对食品安全意识的提高，对于食品中有毒有害物质的重视程度也在逐渐提升。含氮化合物中的氰化物作为食品中对危害性强的物质之一，对其检测监控尤为重要。高粱籽粒中氰化物的毒性来源于氰苷的水解，而氰苷主要存在于高粱的籽粒中，氰苷本身无毒，当受到破坏时生成醇腈，并在酶的作用下裂解产生毒性。高粱籽粒中的氰化物对人体健康具有一定的危害，主要表现为：氰化物可与血红蛋白结合，影响氧的传递，导致缺氧症状，如头晕、乏力等。因此，为了保障人体健康，需要对高粱籽粒中的氰化物进行监测。With the improvement of people's awareness of food safety, the degree of attention to toxic and harmful substances in food is gradually increasing. As one of the most harmful substances in food, cyanide in nitrogen-containing compounds is particularly important for its detection and monitoring. The toxicity of cyanide in sorghum grains comes from the hydrolysis of cyanogenic glycosides, which mainly exist in sorghum grains. The cyanogenic glycosides themselves are non-toxic, and when destroyed, they form alcohol nitriles, which are cleaved by enzymes to produce toxicity. Cyanide in sorghum grains has certain hazards to human health. The main manifestations are: cyanide can combine with hemoglobin, affect the transmission of oxygen, and cause symptoms of hypoxia, such as dizziness and fatigue. Therefore, in order to protect human health, it is necessary to monitor the cyanide in sorghum grain.
目前，针对食物中的氰化物含量的检测，有以下几种方法：烘干法，将高粱籽粒烘干后，用水浸泡一段时间，然后用碘液测定其氰化物含量，这种方法简单易行，但精度较低，不适用于大规模测定；分光光度法，该方法不适用于高粱中氰化物含量的检测，因为在提取高粱中的氰化物的同时，也会把高粱中的色素等带有颜色的物质提取出来，用分光光度计检测时会产生干扰，而且前处理繁琐，时间较长，重复性较差；定性法，这种方法只能确定氰化物的存在，却不能确定高粱中氰化物的具体含量。At present, there are several methods for the detection of cyanide content in food: the drying method, after drying the sorghum grains, soaking them in water for a period of time, and then measuring the cyanide content with iodine solution, this method is simple and easy , but the accuracy is low, not suitable for large-scale determination; spectrophotometry, this method is not suitable for the detection of cyanide content in sorghum, because when extracting cyanide in sorghum, it will also bring pigments in sorghum, etc. The extracted colored substances will cause interference when detected by a spectrophotometer, and the pretreatment is cumbersome, the time is long, and the repeatability is poor; qualitative method, this method can only determine the existence of cyanide, but cannot determine the presence of cyanide in sorghum. Specific content of cyanide.
因此，提供一种能更加准确、简便的检测高粱中氰化物含量的方法是本领域技术人员亟需解决的问题。Therefore, it is an urgent problem for those skilled in the art to provide a more accurate and convenient method for detecting the content of cyanide in sorghum.
发明内容Contents of the invention
本发明针对目前存在的问题，能够更加快速准确的检测高粱中氰化物含量，本申请提供一种快速检测方法。同时该方法也具有较高的灵敏度和准确度，具有较强的抗干扰能力，重现性好。本发明所述的含氮化合物为氰化物。The present invention aims at the existing problems and can detect the content of cyanide in sorghum more rapidly and accurately, and the present application provides a rapid detection method. At the same time, the method also has high sensitivity and accuracy, strong anti-interference ability and good reproducibility. The nitrogen-containing compound described in the present invention is cyanide.
本发明提供了一种高粱中含氮化合物含量的测定方法，所述方法具体包括以下步骤：The invention provides a method for determining the content of nitrogen-containing compounds in sorghum, and the method specifically includes the following steps:
(1)样品制备：收集高粱籽粒后风干，再研磨成粉末状，制得高粱样品；(1) Sample preparation: air-dry after collecting sorghum grains, and then grind them into powder to obtain sorghum samples;
(2)样品前处理：称取高粱样品至样品瓶内，加入氢氧化钠溶液，振荡提取20～40min，超声处理15～25min，放入35～45℃水浴中提取7～9h，离心后取上层清液至顶空瓶中，分别加入磷酸和氯胺T衍生，然后在45～55℃条件下顶空平衡20～35min；(2) Sample pretreatment: Weigh the sorghum sample into a sample bottle, add sodium hydroxide solution, shake and extract for 20-40 minutes, ultrasonically treat for 15-25 minutes, put it in a 35-45°C water bath for extraction for 7-9 hours, and take it after centrifugation. Put the supernatant into the headspace bottle, add phosphoric acid and chloramine T to derivatize, and then equilibrate the headspace at 45-55°C for 20-35 minutes;
(3)检测分析：取步骤(3)中顶空平衡后的样品注入到冷阱调制器进行冷阱富集后，再以色谱-四级杆质谱仪进行检测；(3) Detection and analysis: take the sample after headspace equilibrium in step (3) and inject it into the cold trap modulator for cold trap enrichment, and then detect it with chromatography-quadrupole mass spectrometer;
(4)采用氰化氢标准物质进行定性确认，高分辨选择离子外标法进行定量分析。(4) The hydrogen cyanide standard substance was used for qualitative confirmation, and the high-resolution selected ion external standard method was used for quantitative analysis.
进一步的，在步骤(2)中，所取高粱样品质量与所述样品瓶体积之比为0.5g：(3～6)ml。Further, in step (2), the ratio of the mass of the sorghum sample taken to the volume of the sample bottle is 0.5 g: (3-6) ml.
优选的，在步骤(2)中，所取高粱样品质量与所述样品瓶体积之比为0.5g：5ml。Preferably, in step (2), the ratio of the mass of the sorghum sample taken to the volume of the sample bottle is 0.5g:5ml.
进一步的，在步骤(2)中，所加入的氢氧化钠溶液为0.1％氢氧化钠水溶液。Further, in step (2), the sodium hydroxide solution added is 0.1% sodium hydroxide aqueous solution.
进一步的，在步骤(2)中，上层清液取样体积和顶空瓶体积之比为1：(18～22)mL。Further, in step (2), the ratio of the sampling volume of the supernatant to the volume of the headspace bottle is 1: (18-22) mL.
优选的，在步骤(2)中上层清液取样体积和顶空瓶体积之比为1：20mL。Preferably, in step (2), the ratio of the sampling volume of the supernatant to the volume of the headspace bottle is 1:20mL.
进一步的，在步骤(2)中，所述氯胺T的溶度为10g/L。Further, in step (2), the solubility of the chloramine T is 10g/L.
进一步的，在步骤(2)中上层清液取样体积和磷酸的体积比是1：(0.08～0.12)。Further, in step (2), the volume ratio of the sampling volume of the supernatant to phosphoric acid is 1: (0.08-0.12).
进一步的，在步骤(2)中上层清液取样体积和氯胺T的体积比是1：(0.08～0.12)。Further, in step (2), the volume ratio of the sampling volume of the supernatant to the chloramine T is 1: (0.08-0.12).
优选的，在步骤(2)中上层清液取样体积和磷酸的体积比是1：0.1。Preferably, in step (2), the volume ratio of supernatant sample volume to phosphoric acid is 1:0.1.
优选的，在步骤(2)中上层清液取样体积和氯胺T的体积比是1：0.1。Preferably, in step (2), the volume ratio of the sampling volume of the supernatant to the chloramine T is 1:0.1.
进一步的，在步骤(3)中测试条件：Further, test the condition in step (3):
色谱柱为HP-Wax，规格为30m×0.25mm×0.25μm；The chromatographic column is HP-Wax with a specification of 30m×0.25mm×0.25μm;
色谱柱温度：40℃保持10min，后运行至210℃保持3min，调制时间：5min，调制时长：60s；Chromatographic column temperature: keep at 40°C for 10min, then run to 210°C for 3min, modulation time: 5min, modulation time: 60s;
进样口温度：210℃，不分流；载气为氦气，流速恒定为1.0mL/min；Injection port temperature: 210°C, splitless; the carrier gas is helium, and the flow rate is constant at 1.0mL/min;
质谱条件：传输线温度200℃，离子源温度200℃，四级杆温度150℃；Mass spectrometry conditions: transfer line temperature 200°C, ion source temperature 200°C, quadrupole temperature 150°C;
电离模式：EI 70eV，质量范围：35-400m/z。Ionization mode: EI 70eV, mass range: 35-400m/z.
进一步的，所述氰化氢标准物质为50mg/L。Further, the hydrogen cyanide standard substance is 50mg/L.
本发明提供了一种高粱中含氮化合物含量的测定方法，所述方法具体包括以下步骤：The invention provides a method for determining the content of nitrogen-containing compounds in sorghum, and the method specifically includes the following steps:
(1)样品的采集与制备(1) Sample collection and preparation
高粱样品田间种植过程中套袋处理，收获高粱籽粒样品后自然风干，再使用粉碎机研磨成粉末状，制得高粱样品；The sorghum samples were bagged during the field planting process, the sorghum grain samples were harvested, air-dried naturally, and then ground into powder using a grinder to obtain sorghum samples;
(2)样品前处理(2) Sample pretreatment
称取0.5000g上述高粱样品至5mL样品瓶内，加入4mL 0.1％氢氧化钠水溶液，振荡提取30min，再超声20min，放入40℃水浴中提取8h，离心后取上层清液1mL至20mL顶空瓶中，分别加入0.1mL磷酸和0.1mL氯胺T(10g/L)衍生，然后在50℃条件下顶空平衡30min，再用顶空进样针取1mL进样分析，用气相高分辨质谱仪检测，其中，顶空进样针中的样品先注入到冷阱调制器，再进入气相高分辨质谱仪进行检测。Weigh 0.5000g of the above-mentioned sorghum sample into a 5mL sample bottle, add 4mL of 0.1% sodium hydroxide aqueous solution, shake and extract for 30min, then sonicate for 20min, put it in a 40℃ water bath for extraction for 8h, and take 1mL of supernatant to 20mL headspace after centrifugation Add 0.1mL of phosphoric acid and 0.1mL of chloramine T (10g/L) to the bottle for derivatization, then equilibrate in the headspace for 30min at 50°C, then use a headspace sampling needle to take 1mL of sample for analysis, and use gas phase high-resolution mass spectrometry Instrument detection, wherein the sample in the headspace sampling needle is first injected into the cold trap modulator, and then enters the gas phase high-resolution mass spectrometer for detection.
(3)仪器分析条件(3) Instrument analysis conditions
色谱柱为HP-Wax，规格为30m×0.25mm×0.25μm；The chromatographic column is HP-Wax with a specification of 30m×0.25mm×0.25μm;
色谱柱温度：40℃保持10min，后运行至210℃保持3min，调制时间：5min，调制时长：60s；Chromatographic column temperature: keep at 40°C for 10min, then run to 210°C for 3min, modulation time: 5min, modulation time: 60s;
进样口温度：210℃，不分流；载气为氦气，流速恒定为1.0mL/min；Injection port temperature: 210°C, splitless; the carrier gas is helium, and the flow rate is constant at 1.0mL/min;
质谱条件：传输线温度200℃，离子源温度200℃，四级杆温度150℃；Mass spectrometry conditions: transfer line temperature 200°C, ion source temperature 200°C, quadrupole temperature 150°C;
电离模式：EI 70eV，质量范围：35-400m/z。Ionization mode: EI 70eV, mass range: 35-400m/z.
(4)定性与定量方法(4) Qualitative and quantitative methods
采用氰化氢标准物质进行定性确认，高分辨选择离子外标法进行定量分析；氰化物标准物质：50mg/L。Hydrogen cyanide standard substance is used for qualitative confirmation, and high-resolution selected ion external standard method is used for quantitative analysis; cyanide standard substance: 50mg/L.
本发明所提供的方法在高粱含氮化合物含量测量领域的应用。Application of the method provided by the invention in the field of measuring nitrogenous compound content in sorghum.
本申请实施例中提供的一个或多个技术方案，至少具有如下任一技术效果或优点：One or more technical solutions provided in the embodiments of the present application have at least any of the following technical effects or advantages:
1.在样品检测前，通过衍生化的前处理方法，能够使一些在正常检测器上没有响应或响应值较低的化合物转化为具有特别高效应值的化合物；同时能够除去对仪器或分析系统有害的物质，如强酸或强碱性物质，如生物大分子等，延长仪器使用寿命，使分析测定能长期保持在稳定、可靠的状态下进行。1. Before sample detection, some compounds that have no response or low response value on the normal detector can be converted into compounds with particularly high effect value through the derivatization pretreatment method; Harmful substances, such as strong acid or strong alkaline substances, such as biological macromolecules, etc., prolong the service life of the instrument, so that the analysis and determination can be carried out in a stable and reliable state for a long time.
2.磷酸是一种弱酸，具有良好的溶解性和稳定性，在氰化物衍生化反应中，可以将氰化物转化为氰化物酰胺，从而增强氰化物的检测灵敏度和选择性。2. Phosphoric acid is a weak acid with good solubility and stability. In the cyanide derivatization reaction, cyanide can be converted into cyanide amide, thereby enhancing the detection sensitivity and selectivity of cyanide.
3.氯胺T在氰化物衍生化反应中，可以作为氰化物的还原剂，将氰化物还原为氨气和氰化氢，从而增强氰化物的检测灵敏度和选择性。3. Chloramine T can be used as a reducing agent for cyanide in the cyanide derivatization reaction, reducing cyanide to ammonia gas and hydrogen cyanide, thereby enhancing the detection sensitivity and selectivity of cyanide.
4.本发明提供的针对高粱中含氮化合物含量的检测方法，在低样品量的情况下，快速处理前处理样品，能够提高检测效率，同时该方法也具有较高的灵敏度和准确度，具有较强的抗干扰能力，重现性好。4. The detection method for the content of nitrogen-containing compounds in sorghum provided by the present invention, in the case of low sample volume, can quickly process the pre-treatment sample, which can improve the detection efficiency. At the same time, the method also has higher sensitivity and accuracy, and has Strong anti-interference ability, good reproducibility.
附图说明Description of drawings
图1是本发明中一实施例中高灵敏含氮化合物检测示意图。Fig. 1 is a schematic diagram of highly sensitive nitrogen-containing compound detection in an embodiment of the present invention.
图2是本发明一实施例中八面城样品的气相色谱图。Fig. 2 is a gas chromatogram of the Bamiancheng sample in an embodiment of the present invention.
图3是本发明一实施例中黑色在来种样品的气相色谱图。Fig. 3 is a gas chromatogram of a black sample in an embodiment of the present invention.
图4是本发明一实施例中苏丹草样品的气相色谱图。Fig. 4 is the gas chromatogram of Sudan Grass sample in an embodiment of the present invention.
图5是本发明一实施例中小白粮样品的气相色谱图。Fig. 5 is a gas chromatogram of a small white grain sample in an embodiment of the present invention.
图6是本发明一实施例中小红高粱样品的气相色谱图。Fig. 6 is a gas chromatogram of a small red sorghum sample in an embodiment of the present invention.
图7是本发明一实施例中小粘棒样品的气相色谱图。Fig. 7 is a gas chromatogram of a small sticky stick sample in an embodiment of the present invention.
图8是本发明一实施例中263样品的气相色谱图。Fig. 8 is a gas chromatogram of 263 samples in an embodiment of the present invention.
图9是本发明一实施例中R21样品的气相色谱图。Fig. 9 is a gas chromatogram of the R21 sample in an embodiment of the present invention.
图10是本发明一实施例中高08样品的气相色谱图。Fig. 10 is a gas chromatogram of Gao 08 sample in an embodiment of the present invention.
图11是本发明一实施例中高10样品的气相色谱图。Fig. 11 is a gas chromatogram of the Gao 10 sample in an embodiment of the present invention.
图12是本发明一实施例中R34样品的气相色谱图。Fig. 12 is a gas chromatogram of the R34 sample in an embodiment of the present invention.
图13是本发明一实施例中1522样品的气相色谱图。Fig. 13 is a gas chromatogram of 1522 samples in an embodiment of the present invention.
图14是本发明一实施例中T38样品的气相色谱图。Fig. 14 is a gas chromatogram of the T38 sample in an embodiment of the present invention.
图15是本发明一实施例中16样品的气相色谱图。Fig. 15 is a gas chromatogram of 16 samples in an embodiment of the present invention.
图16是本发明一实施例中黔高1号样品的气相色谱图。Fig. 16 is a gas chromatogram of Qiangao No. 1 sample in an embodiment of the present invention.
图17是本发明一实施例中标准样品的气相色谱图。Fig. 17 is a gas chromatogram of a standard sample in an embodiment of the present invention.
具体实施方式Detailed ways
本发明申请中的含氮化合物为氰化物。下面结合实施例来说明本发明的具体实施方式，但以下实施例只是用来详细说明本发明，并不以任何方式限制本发明的范围。The nitrogen-containing compounds in the application of the present invention are cyanides. The specific implementation of the present invention will be described below in conjunction with the examples, but the following examples are only used to describe the present invention in detail, and do not limit the scope of the present invention in any way.
在以下实施例中所涉及的仪器设备如无特别说明，均为常规仪器设备；所涉及的生化试剂和试验材料如无特别说明，均为市售产品；所涉及的试验方法，如无特别说明，均为常规方法。The instruments and equipment involved in the following examples are conventional instruments and equipment unless otherwise specified; the involved biochemical reagents and test materials are commercially available products unless otherwise specified; the involved test methods are all commercially available unless otherwise specified , are conventional methods.
本发明实施例中的使用的仪器：气相色谱四级杆飞行时间质谱联用仪(美国Agilent，7890B-7250)，并配置固态热调制器(上海雪景，SSM1800)和三合一自动进样器(瑞士CTC，PAL RSI120)；冷阱调制器(雪景科技，SM1800)；电子天平(美国Mettler-toledo，AL-104)以及其他常用玻璃仪器。The instrument used in the embodiment of the present invention: gas chromatography quadrupole time-of-flight mass spectrometer (Agilent, 7890B-7250 in the United States), and configures a solid-state thermal modulator (Shanghai Xuejing, SSM1800) and a three-in-one autosampler (Switzerland CTC, PAL RSI120); cold trap modulator (Snow Technology, SM1800); electronic balance (US Mettler-toledo, AL-104) and other commonly used glass instruments.
实施例一Embodiment one
(1)样品的采集与制备(1) Sample collection and preparation
高粱样品田间种植过程中套袋处理，收获高粱籽粒样品后自然风干，再使用粉碎机研磨成粉末状，制得高粱样品；The sorghum samples were bagged during the field planting process, the sorghum grain samples were harvested, air-dried naturally, and then ground into powder using a grinder to obtain sorghum samples;
(2)样品前处理(2) Sample pretreatment
称取0.5000g上述高粱样品至5mL样品瓶内，加入4mL 0.1％氢氧化钠水溶液，振荡提取30min，再超声20min，放入40℃水浴中提取8h，离心后取上层清液1mL至20mL顶空瓶中，分别加入0.1mL磷酸和0.1mL氯胺T(10g/L)衍生，然后在50℃条件下顶空平衡30min，再用顶空进样针取1mL进样分析，用气相高分辨质谱仪检测，其中，顶空进样针中的样品先注入到冷阱调制器，再进入气相高分辨质谱仪进行检测(如图1)。Weigh 0.5000g of the above-mentioned sorghum sample into a 5mL sample bottle, add 4mL of 0.1% sodium hydroxide aqueous solution, shake and extract for 30min, then sonicate for 20min, put it in a 40℃ water bath for extraction for 8h, and take 1mL of supernatant to 20mL headspace after centrifugation Add 0.1mL of phosphoric acid and 0.1mL of chloramine T (10g/L) to the bottle for derivatization, then equilibrate in the headspace for 30min at 50°C, then use a headspace sampling needle to take 1mL of sample for analysis, and use gas phase high-resolution mass spectrometry Instrument detection, wherein, the sample in the headspace sampling needle is first injected into the cold trap modulator, and then enters the gas phase high-resolution mass spectrometer for detection (as shown in Figure 1).
(3)仪器分析条件(3) Instrument analysis conditions
色谱柱为HP-Wax，规格为30m×0.25mm×0.25μm；The chromatographic column is HP-Wax with a specification of 30m×0.25mm×0.25μm;
色谱柱温度：40℃保持10min，后运行至210℃保持3min，调制时间：5min，调制时长：60s；Chromatographic column temperature: keep at 40°C for 10min, then run to 210°C for 3min, modulation time: 5min, modulation time: 60s;
进样口温度：210℃，不分流；载气为氦气，流速恒定为1.0mL/min；Injection port temperature: 210°C, splitless; the carrier gas is helium, and the flow rate is constant at 1.0mL/min;
质谱条件：传输线温度200℃，离子源温度200℃，四级杆温度150℃；Mass spectrometry conditions: transfer line temperature 200°C, ion source temperature 200°C, quadrupole temperature 150°C;
电离模式：EI 70eV，质量范围：35-400m/z。Ionization mode: EI 70eV, mass range: 35-400m/z.
(4)定性与定量方法(4) Qualitative and quantitative methods
采用氰化氢标准(中国计量院，50mg/L)物质进行定性确认，高分辨选择离子外标法进行定量分析；氰化物标准物质：50mg/L(中国计量科学院)。Hydrogen cyanide standard (National Institute of Metrology, 50mg/L) was used for qualitative confirmation, and high-resolution selected ion external standard method was used for quantitative analysis; cyanide standard substance: 50mg/L (National Institute of Metrology).
(5)具体检测应用实例(5) Specific detection application examples
选取不同种类的高粱样品，分别是青壳洋；赤水红粱1号；赤水红粱2号；红台粱；茅红糯2号；遵红1301；红茅糯2号；茅红糯1号；小缨子；红珍珠；黔高2号；黔高4号；黔高7号；黔高8号；黔高9号；黔高10号；红粱丰21-1；红粱丰21-2；红粱丰21-3；红粱丰21-4；红粱丰21-5；红粱丰21-6；红粱丰21-7，按照上述步骤进行测定，数据记录及分析如下：Different types of sorghum samples were selected, namely Qingkeyang; Chishui Hongliang No. 1; Chishui Hongliang No. 2; Hongtailiang; Maohongnuo No. 2; Zunhong 1301; ; Xiaoyingzi; Red Pearl; Qiangao No. 2; Qiangao No. 4; Qiangao No. 7; Qiangao No. 8; Qiangao No. 9; Qiangao No. 10; Hongliangfeng 21-3; Hongliangfeng 21-4; Hongliangfeng 21-5; Hongliangfeng 21-6;
实施例二Embodiment two
(1)样品的采集与制备(1) Sample collection and preparation
高粱样品田间种植过程中套袋处理，收获高粱籽粒样品后自然风干，在使用粉碎机研磨成粉末状。The sorghum samples were bagged during field planting, and the sorghum grain samples were harvested and air-dried, and then ground into powder using a grinder.
(2)样品前处理(2) Sample pretreatment
称取0.5000g上述样品至5mL样品瓶内，加入4mL 0.1％氢氧化钠水溶液，振荡提取30min，再超声20min，放入40℃水浴中提取8h，离心后取上层清液1mL至20mL顶空瓶中，分别加入0.1mL磷酸和0.1mL氯胺T(10g/L)衍生，然后在50℃条件下顶空平衡30min，再用顶空进样针取1mL进样分析，用气相高分辨质谱仪检测，其中，顶空进样针中的样品先注入到冷阱调制器，再进入气相高分辨质谱仪进行检测。Weigh 0.5000g of the above sample into a 5mL sample bottle, add 4mL of 0.1% sodium hydroxide aqueous solution, shake and extract for 30min, then sonicate for 20min, put it in a 40°C water bath for extraction for 8h, and after centrifugation, take 1mL of the supernatant to a 20mL headspace bottle Add 0.1mL of phosphoric acid and 0.1mL of chloramine T (10g/L) to derivatize, and then equilibrate in the headspace for 30min at 50°C, then use a headspace sampling needle to take 1mL of sample for analysis, and use a gas phase high-resolution mass spectrometer Detection, wherein the sample in the headspace sampling needle is first injected into the cold trap modulator, and then enters the gas phase high-resolution mass spectrometer for detection.
(3)仪器分析条件(3) Instrument analysis conditions
色谱柱为HP-Wax，规格为30m×0.25mm×0.25μm；The chromatographic column is HP-Wax with a specification of 30m×0.25mm×0.25μm;
色谱柱温度：40℃保持10min，后运行至210℃保持3min，调制时间：5min，调制时长：60s；Chromatographic column temperature: keep at 40°C for 10min, then run to 210°C for 3min, modulation time: 5min, modulation time: 60s;
进样口温度：210℃，不分流；载气为氦气，流速恒定为1.0mL/min；Injection port temperature: 210°C, splitless; the carrier gas is helium, and the flow rate is constant at 1.0mL/min;
质谱条件：传输线温度200℃，离子源温度200℃，四级杆温度150℃；Mass spectrometry conditions: transfer line temperature 200°C, ion source temperature 200°C, quadrupole temperature 150°C;
电离模式：EI 70eV，质量范围：35-400m/z。Ionization mode: EI 70eV, mass range: 35-400m/z.
(4)定性与定量方法(4) Qualitative and quantitative methods
采用氰化氢标准(中国计量院，50mg/L)物质进行定性确认，高分辨选择离子外标法进行定量分析；氰化物标准物质：50mg/L(中国计量科学院)。Hydrogen cyanide standard (National Institute of Metrology, 50mg/L) was used for qualitative confirmation, and high-resolution selected ion external standard method was used for quantitative analysis; cyanide standard substance: 50mg/L (National Institute of Metrology).
(5)具体检测应用实例(5) Specific detection application examples
选取不同品种的高粱籽粒样品，分别是八面城；黑色在来种；苏丹草；小白粮；小红高粱；小粘棒；263；R21；高08；高10；R34；1522；T38；16；黔高1号，按照上述步骤进行3次独立重复测定，数据记录及分析如下：Sorghum grain samples of different varieties were selected, namely Bamiancheng; Black Zalaizhong; Sudan Grass; Xiaobailiang; Xiaohong Sorghum; 16; Qiangao No. 1, follow the above steps to carry out 3 independent repeated measurements, the data records and analysis are as follows:
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者同等替换，而不脱离本发明技术方案的实质和范围。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that The technical solution of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solution of the present invention.
| Application Number | Priority Date | Filing Date | Title |
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| CN202310465339.8ACN116609452A (en) | 2023-04-26 | 2023-04-26 | A method for determining the content of nitrogen-containing compounds in sorghum grains |
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| CN202310465339.8ACN116609452A (en) | 2023-04-26 | 2023-04-26 | A method for determining the content of nitrogen-containing compounds in sorghum grains |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112881548A (en)* | 2021-01-12 | 2021-06-01 | 济南趵突泉酿酒有限责任公司 | Method for rapidly detecting cyanide in sorghum |
| CN115166106A (en)* | 2021-11-26 | 2022-10-11 | 国家食品安全风险评估中心 | Method for detecting cyanide content in white spirit or white spirit fermentation process sample |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112881548A (en)* | 2021-01-12 | 2021-06-01 | 济南趵突泉酿酒有限责任公司 | Method for rapidly detecting cyanide in sorghum |
| CN115166106A (en)* | 2021-11-26 | 2022-10-11 | 国家食品安全风险评估中心 | Method for detecting cyanide content in white spirit or white spirit fermentation process sample |
| Title |
|---|
| 刘宇;赵晶;张欣;于波;权伍英;: "顶空气相色谱法测定粮食中的氰化物", 中国卫生检验杂志, no. 03, 31 March 2009 (2009-03-31), pages 552 - 553* |
| 徐毅;龚文杰;陈海燕;: "坚果中微量氰化物的顶空气相色谱法测定", 中国卫生检验杂志, no. 12, 31 December 2020 (2020-12-31), pages 1432 - 1434* |
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