CN116256442A - A method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres - Google Patents
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Abstract
Translated fromChinese
Description
Translated fromChinese技术领域technical field
本申请涉及栓塞微球检测技术领域，具体而言，涉及一种聚乙烯醇栓塞微球中含碘化合物的检测方法。The present application relates to the technical field of detection of embolic microspheres, in particular to a method for detecting iodine-containing compounds in polyvinyl alcohol embolic microspheres.
背景技术Background technique
由于碘原子对X射线的强吸收，含碘化合物，尤其是含碘有机化合物，可在X射线检测下人体内显影。Due to the strong absorption of iodine atoms to X-rays, iodine-containing compounds, especially iodine-containing organic compounds, can be developed in the human body under X-ray detection.
2，3，5-三碘苯甲酰胺作为显影聚乙烯醇微球合成过程中产生的副产物，在合成修饰过程中，可能会产生残留，影响到产品安全性，因此需要检测聚乙烯醇微球中的2，3，5-三碘苯甲酰胺的含量。2,3,5-Triiodobenzamide is a by-product produced during the synthesis of developed polyvinyl alcohol microspheres. During the synthesis modification process, residues may be produced, which will affect product safety. Therefore, it is necessary to detect polyvinyl alcohol microspheres. The content of 2,3,5-triiodobenzamide in the ball.
发明内容Contents of the invention
本申请提供了一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其能够将含碘化合物尽可能的从栓塞微球中提取出来，提高检测的灵敏度。The present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolic microspheres, which can extract as much iodine-containing compounds from embolic microspheres as possible to improve detection sensitivity.
本申请的实施例是这样实现的：The embodiment of the application is realized like this:
在第一方面，本申请示例提供了一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括：In a first aspect, the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes:
S1、将干燥后的聚乙烯醇栓塞微球和溶剂混合制得混合物，使混合物在40℃～60℃下浸提至少2h，得到待测样品。S1. Mix the dried polyvinyl alcohol embolization microspheres with a solvent to prepare a mixture, and extract the mixture at 40° C. to 60° C. for at least 2 hours to obtain a sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量，流动相包括水相和有机相。S2. Detect the content of the iodine-containing compound in the sample to be tested by high performance liquid chromatography, and the mobile phase includes an aqueous phase and an organic phase.
在上述技术方案中，本申请的聚乙烯醇栓塞微球中含碘化合物的检测方法通过干燥聚乙烯醇栓塞微球以及控制浸提温度、浸提时间，能够尽可能的从栓塞微球中提取出含碘化合物，从而提高检测的灵敏度。高效液相色谱法能够检测含碘化合物的含量。In the above technical scheme, the detection method of the iodine-containing compound in the polyvinyl alcohol embolization microspheres of the present application can extract as much as possible from the embolization microspheres by drying the polyvinyl alcohol embolization microspheres and controlling the extraction temperature and extraction time. out iodine-containing compounds, thereby improving the sensitivity of detection. High performance liquid chromatography can detect the content of iodine-containing compounds.
结合第一方面，在本申请的第一方面的第一种可能的示例中，含碘化合物为2，3，5-三碘苯甲酰胺。With reference to the first aspect, in the first possible example of the first aspect of the present application, the iodine-containing compound is 2,3,5-triiodobenzamide.
在上述示例中，2，3，5-三碘苯甲酰胺具有苯甲酰胺结构，其具有较好的紫外吸收，高效液相色谱法能够检测其含量。In the above example, 2,3,5-triiodobenzamide has a benzamide structure, which has good ultraviolet absorption, and its content can be detected by high performance liquid chromatography.
结合第一方面，在本申请的第一方面的第二种可能的示例中，使混合物在50℃下浸提至少2h。In conjunction with the first aspect, in a second possible example of the first aspect of the present application, the mixture is leached at 50° C. for at least 2 h.
可选地，在浸提过程中，使混合物保持振摇状态。Optionally, the mixture is kept shaken during the leaching process.
在上述示例中，在浸提过程中使混合物保持振摇状态能够提高2，3，5-三碘苯甲酰胺的浸出率，从而提高检测的灵敏度。In the above example, keeping the mixture in a shaken state during the leaching process can increase the leaching rate of 2,3,5-triiodobenzamide, thereby improving the detection sensitivity.
结合第一方面，在本申请的第一方面的第三种可能的示例中，上述干燥后的聚乙烯醇栓塞微球通过以下方法获得：In combination with the first aspect, in the third possible example of the first aspect of the present application, the above-mentioned dried polyvinyl alcohol embolization microspheres are obtained by the following method:
将聚乙烯醇栓塞微球在50℃～70℃下干燥1.5～2.5h。The polyvinyl alcohol embolic microspheres are dried at 50° C. to 70° C. for 1.5 to 2.5 hours.
可选地，将聚乙烯醇栓塞微球在60℃下干燥2h。Optionally, dry the polyvinyl alcohol embolization microspheres at 60 °C for 2 h.
结合第一方面，在本申请的第一方面的第四种可能的示例中，上述干燥后的聚乙烯醇栓塞微球和溶剂的质量体积比为100mg:1mL～3mL。With reference to the first aspect, in a fourth possible example of the first aspect of the present application, the mass-volume ratio of the above-mentioned dried polyvinyl alcohol embolization microspheres to the solvent is 100 mg:1 mL˜3 mL.
干燥后的聚乙烯醇栓塞微球和溶剂的质量体积比为100mg:2mL。The mass-volume ratio of the dried polyvinyl alcohol embolization microspheres to the solvent was 100mg:2mL.
结合第一方面，在本申请的第一方面的第五种可能的示例中，上述溶剂为二甲基亚砜。With reference to the first aspect, in a fifth possible example of the first aspect of the present application, the above-mentioned solvent is dimethyl sulfoxide.
在上述示例中，2，3，5-三碘苯甲酰胺在二甲基亚砜中的溶解度较高。In the above example, 2,3,5-triiodobenzamide has a high solubility in DMSO.
结合第一方面，在本申请的第一方面的第六种可能的示例中，上述含碘化合物的检测波长为245nm。With reference to the first aspect, in a sixth possible example of the first aspect of the present application, the detection wavelength of the above-mentioned iodine-containing compound is 245 nm.
结合第一方面，在本申请的第一方面的第七种可能的示例中，高效液相色谱法中色谱柱填料为C18烷基硅胶。With reference to the first aspect, in the seventh possible example of the first aspect of the present application, the chromatographic column filler in high performance liquid chromatography is C18 alkyl silica gel.
可选地，色谱柱的直径为4.6mm，色谱柱的长度为250mm，填料的粒径为5.0μm。Optionally, the diameter of the chromatographic column is 4.6 mm, the length of the chromatographic column is 250 mm, and the particle diameter of the filler is 5.0 μm.
结合第一方面，在本申请的第一方面的第八种可能的示例中，上述水相为0.1wt％磷酸水溶液，有机相为甲醇。With reference to the first aspect, in the eighth possible example of the first aspect of the present application, the above-mentioned aqueous phase is a 0.1 wt% phosphoric acid aqueous solution, and the organic phase is methanol.
可选地，流动相的流速为1mL/min。Optionally, the flow rate of the mobile phase is 1 mL/min.
结合第一方面，在本申请的第一方面的第九种可能的示例中，上述高效液相色谱法的洗脱程序为：In conjunction with the first aspect, in the ninth possible example of the first aspect of the present application, the elution procedure of the above high performance liquid chromatography is:
S1、洗杂，流速为1mL/min，时间为5min，水相：有机相由50％:50％线性拉到10％:90％。S1. Washing impurities, the flow rate is 1mL/min, the time is 5min, and the water phase: organic phase is linearly pulled from 50%:50% to 10%:90%.
S2、洗脱，流速为1mL/min，时间为7min，水相：有机相为10％:90％。S2, elution, flow rate is 1mL/min, time is 7min, aqueous phase: organic phase is 10%:90%.
附图说明Description of drawings
为了更清楚地说明本申请实施例的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本申请的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。In order to more clearly illustrate the technical solutions of the embodiments of the present application, the accompanying drawings that are required in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present application, and thus It should be regarded as a limitation on the scope, and those skilled in the art can also obtain other related drawings based on these drawings without creative work.
图1为本申请实施例中溶剂为DMSO的高效液相色谱法检测得到的色谱图；Fig. 1 is the chromatogram that the high performance liquid chromatography detection that solvent is DMSO in the embodiment of the application obtains;
图2为本申请实施例1中高效液相色谱法检测得到的色谱图；Fig. 2 is the chromatogram that high performance liquid chromatography detects in the
图3为本申请实施例2中高效液相色谱法检测得到的色谱图；Fig. 3 is the chromatogram that high performance liquid chromatography detects in the
图4为本申请实施例3中高效液相色谱法检测得到的色谱图；Fig. 4 is the chromatogram that high performance liquid chromatography detects in the
图5为本申请实施例4中高效液相色谱法检测得到的色谱图；Fig. 5 is the chromatogram that high performance liquid chromatography detects in the
图6为本申请实施例5中高效液相色谱法检测得到的色谱图；Fig. 6 is the chromatogram that high performance liquid chromatography detects in the
图7为本申请实施例6中高效液相色谱法检测得到的色谱图；Fig. 7 is the chromatogram that high performance liquid chromatography detects in the
图8为本申请实施例7中高效液相色谱法检测得到的色谱图；Fig. 8 is the chromatogram that high performance liquid chromatography detects in the
图9为本申请实施例8中高效液相色谱法检测得到的色谱图；Fig. 9 is the chromatogram that high performance liquid chromatography detects in the
图10为本申请对比例1中高效液相色谱法检测得到的色谱图；Fig. 10 is the chromatogram obtained by high performance liquid chromatography detection in comparative example 1 of the present application;
图11为本申请对比例2中高效液相色谱法检测得到的色谱图；Fig. 11 is the chromatogram obtained by high performance liquid chromatography detection in comparative example 2 of the present application;
图12为本申请对比例3中高效液相色谱法检测得到的色谱图；Fig. 12 is the chromatogram obtained by high performance liquid chromatography detection in comparative example 3 of the present application;
图13为本申请对比例4中高效液相色谱法检测得到的色谱图。Fig. 13 is a chromatogram obtained by high performance liquid chromatography in Comparative Example 4 of the present application.
具体实施方式Detailed ways
下面将结合实施例对本申请的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施例仅用于说明本申请，而不应视为限制本申请的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。Embodiments of the present application will be described in detail below in conjunction with examples, but those skilled in the art will understand that the following examples are only used to illustrate the present application, and should not be considered as limiting the scope of the present application. Those who do not indicate the specific conditions in the examples are carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used were not indicated by the manufacturer, and they were all conventional products that could be purchased from the market.
以下针对本申请实施例的一种聚乙烯醇栓塞微球中含碘化合物的检测方法进行具体说明：The following is a specific description of the detection method of iodine-containing compounds in a polyvinyl alcohol embolization microsphere of the embodiment of the present application:
本申请提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括：The application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球干燥成干球。Dry the polyvinyl alcohol embolization microspheres into dry balls.
干燥的温度较低可能导致聚乙烯醇栓塞微球的干燥效果不好，干燥的温度较高可能导致聚乙烯醇栓塞微球变性或破裂。Low drying temperature may lead to poor drying effect of polyvinyl alcohol embolization microspheres, and high drying temperature may cause denaturation or rupture of polyvinyl alcohol embolization microspheres.
干燥包括将聚乙烯醇栓塞微球在50℃～70℃下干燥1.5～2.5h。The drying includes drying the polyvinyl alcohol embolic microspheres at 50° C. to 70° C. for 1.5 to 2.5 hours.
作为示例，干燥可以包括将聚乙烯醇栓塞微球在50℃、55℃、60℃、65℃或70℃下干燥1.5h、2h或2.5h。As an example, drying may include drying the polyvinyl alcohol embolic microspheres at 50°C, 55°C, 60°C, 65°C or 70°C for 1.5h, 2h or 2.5h.
可选地，干燥包括将聚乙烯醇栓塞微球在60℃下干燥2h。Optionally, the drying includes drying the polyvinyl alcohol embolization microspheres at 60° C. for 2 hours.
将干燥后的聚乙烯醇栓塞微球和溶剂混合制得混合物，使混合物在40℃～60℃下浸提至少2h，得到待测样品。The dried polyvinyl alcohol embolization microspheres are mixed with a solvent to prepare a mixture, and the mixture is leached at 40° C. to 60° C. for at least 2 hours to obtain a sample to be tested.
含碘化合物为2，3，5-三碘苯甲酰胺。The iodine-containing compound is 2,3,5-triiodobenzamide.
干燥后的聚乙烯醇栓塞微球和溶剂的质量体积比为100mg:1mL～3mL。The mass-volume ratio of the dried polyvinyl alcohol embolization microspheres to the solvent is 100mg:1mL-3mL.
作为示例，干燥后的聚乙烯醇栓塞微球和溶剂的质量体积比可以为100mg:1mL、100mg:1.5mL、100mg:2mL、100mg:2.5mL或100mg:3mL。As an example, the mass-volume ratio of the dried polyvinyl alcohol embolization microspheres to the solvent can be 100mg:1mL, 100mg:1.5mL, 100mg:2mL, 100mg:2.5mL or 100mg:3mL.
可选地，干燥后的聚乙烯醇栓塞微球和溶剂的质量体积比为100mg:2mL。Optionally, the mass-volume ratio of the dried polyvinyl alcohol embolization microspheres to the solvent is 100mg:2mL.
作为示例，可以使混合物在40℃、45℃、50℃、55℃或60℃下浸提2h、2.5h或3h。As an example, the mixture may be leached at 40°C, 45°C, 50°C, 55°C or 60°C for 2h, 2.5h or 3h.
可选地，混合物在50℃下浸提至少2h。Optionally, the mixture is leached at 50 °C for at least 2 h.
可选地，在浸提过程中，使混合物保持振摇状态。Optionally, the mixture is kept shaken during the leaching process.
在浸提过程中使混合物保持振摇状态能够提高2，3，5-三碘苯甲酰胺的浸出率，从而提高检测的灵敏度。Keeping the mixture in a shaking state during the leaching process can increase the leaching rate of 2,3,5-triiodobenzamide, thereby improving the detection sensitivity.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
由于2，3，5-三碘苯甲酰胺具有苯甲酰胺结构，其具有较好的紫外吸收，高效液相色谱法能够检测其含量。Since 2,3,5-triiodobenzamide has a benzamide structure, it has good ultraviolet absorption, and its content can be detected by high performance liquid chromatography.
高效液相色谱法检测方法包括：采用C18烷基硅胶色谱柱，流动相以柱流速为1mL/min进行冲洗，流动相包括水相和有机相，前5分钟线性洗杂(水相50％→10％)洗杂，梯度洗脱7min，水相10％，并采用紫外检测器检测，2，3，5-三碘苯甲酰胺的检测波长为245nm。The detection method of high performance liquid chromatography includes: using C18 alkyl silica gel chromatographic column, the mobile phase is washed with a column flow rate of 1mL/min, the mobile phase includes aqueous phase and organic phase, and the first 5 minutes are linearly washed (
可选地，C18烷基硅胶色谱柱包括安捷伦C18烷基硅胶色谱柱。Optionally, the C18 alkyl silica gel chromatography column includes Agilent C18 alkyl silica gel chromatography column.
可选地，色谱柱的直径为4.6mm，色谱柱的长度为250mm，填料的粒径为5.0μm。Optionally, the diameter of the chromatographic column is 4.6 mm, the length of the chromatographic column is 250 mm, and the particle diameter of the filler is 5.0 μm.
水相为0.1wt％磷酸水溶液。The aqueous phase is 0.1 wt% phosphoric acid aqueous solution.
有机相为甲醇。The organic phase is methanol.
可选地，紫外检测器包括DAD检测器。Optionally, the ultraviolet detector comprises a DAD detector.
本申请的聚乙烯醇栓塞微球中含碘化合物的检测方法通过干燥聚乙烯醇栓塞微球以及控制浸提温度、浸提时间，能够尽可能的从栓塞微球中提取出2，3，5-三碘苯甲酰胺，从而提高检测的灵敏度。The method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres of the present application can extract 2, 3, and 5 - Triiodobenzamide, thereby improving the sensitivity of detection.
浸提溶剂筛选Extraction solvent screening
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜(DMSO)(2ml水或2ml甲醇或2ml乙腈)混合制得混合物，使混合物在50℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolism microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls. Take 100 mg of dry balls and mix them with 2 mL of dimethyl sulfoxide (DMSO) (2 mL of water or 2 mL of methanol or 2 mL of acetonitrile) The mixture was prepared, and the mixture was statically leached in a water bath at 50°C for 2 hours to obtain a sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
采用安捷伦C18烷基硅胶色谱柱(规格：4.6*250mm，5.0μm)，流速1mL/min，流动相包括水相和有机相，水相为0.1wt％磷酸水溶液，有机相为甲醇，高效液相洗脱程序为：Agilent C18 alkyl silica gel chromatography column (specification: 4.6*250mm, 5.0μm) is used, the flow rate is 1mL/min, the mobile phase includes aqueous phase and organic phase, the aqueous phase is 0.1wt% phosphoric acid aqueous solution, the organic phase is methanol, and the high performance liquid phase The elution procedure is:
洗脱，流速1mL/min，时间12min，水相：有机相由50％：50％线性拉到10％：90％。Elution, flow rate 1mL/min, time 12min, aqueous phase: organic phase linearly pulled from 50%: 50% to 10%: 90%.
并采用DAD检测器检测，2，3，5-三碘苯甲酰胺的检测波长为245nm。And adopt DAD detector to detect, the detection wavelength of 2,3,5-triiodobenzamide is 245nm.
检测结果如表1，且溶剂为DMSO的高效液相色谱法检测得到的色谱图如图1所示。The test results are shown in Table 1, and the chromatogram obtained by the high-performance liquid chromatography with DMSO as the solvent is shown in Figure 1.
表1不同浸提溶剂的检测结果Table 1 The detection results of different extraction solvents
以下结合实施例对本申请的一种聚乙烯醇栓塞微球中含碘化合物的检测方法作进一步的详细描述。A method for detecting iodine-containing compounds in polyvinyl alcohol embolic microspheres of the present application will be further described in detail in conjunction with the examples below.
实施例1Example 1
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
采用安捷伦C18烷基硅胶色谱柱(规格：4.6*250mm，5.0μm)，流速1mL/min，流动相包括水相和有机相，水相为0.1wt％磷酸水溶液，有机相为甲醇，高效液相洗脱程序为：Agilent C18 alkyl silica gel chromatography column (specification: 4.6*250mm, 5.0μm) is used, the flow rate is 1mL/min, the mobile phase includes aqueous phase and organic phase, the aqueous phase is 0.1wt% phosphoric acid aqueous solution, the organic phase is methanol, and the high performance liquid phase The elution procedure is:
1)洗杂，流速1mL/min，时间5min，水相：有机相由50％：50％线性拉到10％：90％；1) Wash impurities, flow rate 1mL/min, time 5min, water phase: organic phase linearly pulled from 50%: 50% to 10%: 90%;
2)洗脱，流速1mL/min，时间7min，水相：有机相为10％：90％。2) Elution, flow rate 1mL/min, time 7min, aqueous phase:
并采用DAD检测器检测，2，3，5-三碘苯甲酰胺的检测波长为245nm。And adopt DAD detector to detect, the detection wavelength of 2,3,5-triiodobenzamide is 245nm.
实施例2Example 2
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下振摇浸提2h，得到待测样品。Put the polyvinyl alcohol embolism microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and shake the mixture in a water bath at 50°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
实施例3Example 3
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在60℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolism microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 60°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
实施例4Example 4
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在40℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolism microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls. Take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to make a mixture, and let the mixture stand in a water bath at 40°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
实施例5Example 5
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提3h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 3h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
实施例6Example 6
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在80℃下干燥1h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in an air blast drying oven and dry them at 80°C for 1 hour to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
实施例7Example 7
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序，有机相改为乙腈。Perform the same elution procedure as in Example 1, and change the organic phase to acetonitrile.
实施例8Example 8
本申请实施例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The embodiment of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which includes the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序，有机相改为乙腈，水相改为0.01mol/L磷酸二氢钠。The same elution procedure as in Example 1 was carried out, the organic phase was changed to acetonitrile, and the aqueous phase was changed to 0.01 mol/L sodium dihydrogen phosphate.
对比例1Comparative example 1
本申请对比例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The comparative example of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which comprises the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 2h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
采用安捷伦C18烷基硅胶色谱柱(规格：4.6*250mm，5.0μm)，流速1mL/min，流动相包括水相和有机相，水相为0.1wt％磷酸水溶液，有机相为甲醇，高效液相洗脱程序为：Agilent C18 alkyl silica gel chromatography column (specification: 4.6*250mm, 5.0μm) is used, the flow rate is 1mL/min, the mobile phase includes aqueous phase and organic phase, the aqueous phase is 0.1wt% phosphoric acid aqueous solution, the organic phase is methanol, and the high performance liquid phase The elution procedure is:
洗脱，流速1mL/min，时间12min，水相：有机相由50％：50％线性拉到10％：90％。Elution, flow rate 1mL/min, time 12min, aqueous phase: organic phase linearly pulled from 50%: 50% to 10%: 90%.
并采用DAD检测器检测，2，3，5-三碘苯甲酰胺的检测波长为245nm。And adopt DAD detector to detect, the detection wavelength of 2,3,5-triiodobenzamide is 245nm.
对比例2Comparative example 2
本申请对比例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The comparative example of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which comprises the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在25℃下静置浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand at 25°C to soak Lift for 2h to get the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
对比例3Comparative example 3
本申请对比例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The comparative example of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which comprises the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在25℃下振摇浸提2h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls. Take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and shake the mixture at 25°C. Lift for 2h to get the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
对比例4Comparative example 4
本申请对比例提供一种聚乙烯醇栓塞微球中含碘化合物的检测方法，其包括以下步骤：The comparative example of the present application provides a method for detecting iodine-containing compounds in polyvinyl alcohol embolization microspheres, which comprises the following steps:
S1、从聚乙烯醇栓塞微球中提取含碘化合物制得待测样品S1. Extracting iodine-containing compounds from polyvinyl alcohol embolization microspheres to prepare test samples
将聚乙烯醇栓塞微球置于鼓风干燥箱中在60℃下干燥2h变成干球，取100mg干球和2mL二甲基亚砜混合制得混合物，使混合物在50℃水浴下静置浸提1h，得到待测样品。Put the polyvinyl alcohol embolic microspheres in a forced air drying oven and dry them at 60°C for 2 hours to become dry balls, take 100 mg of dry balls and 2 mL of dimethyl sulfoxide to prepare a mixture, and let the mixture stand in a water bath at 50°C Leach for 1h to obtain the sample to be tested.
S2、采用高效液相色谱法检测待测样品中的含碘化合物的含量S2, adopt high performance liquid chromatography to detect the content of the iodine-containing compound in the sample to be tested
执行与实施例1一样的洗脱程序。The same elution procedure as in Example 1 was carried out.
对比例5Comparative example 5
与实施例1的区别是不进行微球的干燥，其他处理和检测条件不变。The difference from Example 1 is that the microspheres are not dried, and other processing and detection conditions remain unchanged.
试验例1Test example 1
根据实施例1～8和对比例1～5检测得到聚乙烯醇栓塞微球中2，3，5-三碘苯甲酰胺，高效液相色谱法检测得到的色谱图如图2～13所示。其中，实施例1～8和对比例1～5的检测结果(峰面积)如表2所示。According to the detection of Examples 1-8 and Comparative Examples 1-5, 2,3,5-triiodobenzamide in the polyvinyl alcohol embolization microspheres is obtained, and the chromatogram obtained by the high-performance liquid chromatography detection is shown in Figures 2-13 . Wherein, the detection results (peak areas) of Examples 1-8 and Comparative Examples 1-5 are shown in Table 2.
表2实施例1～8和对比例1～5的检测结果(峰面积)The detection result (peak area) of table 2
由实施例1和对比例1对比可知，对比例1采用一步线性洗脱的方式不能将杂质和待检测物很好的区分开，而实施例1的方案能够有效的将待检测物区分开，其他洗脱方式区分度虽有改善但是效果不明显。From the comparison of Example 1 and Comparative Example 1, it can be seen that the one-step linear elution method in Comparative Example 1 cannot distinguish the impurities from the substances to be detected well, while the scheme in Example 1 can effectively distinguish the substances to be detected. Although the discrimination of other elution methods has been improved, the effect is not obvious.
由实施例1和实施例2对比可知，振摇浸提和静置浸提相比，振摇浸提的浸提效果更好，实施例2的检测峰面积相较于实施例1的检测峰面积明显增加。By comparison of Example 1 and Example 2, it can be seen that the shaking extraction is better than the static extraction, and the extraction effect of the shaking extraction is better, and the detection peak area of Example 2 is compared with that of Example 1. area increased significantly.
由实施例1、3～4和对比例2可知，当浸提温度保持在40℃～60℃时，提取效果均较好，实施例1、3～4的检测峰面积均保持较高水平。It can be known from Examples 1, 3-4 and Comparative Example 2 that when the extraction temperature is maintained at 40°C-60°C, the extraction effect is better, and the detection peak areas of Examples 1, 3-4 all maintain a relatively high level.
由实施例1、5和对比例4可知，当浸提时间为2h-3h时，提取效果均较好，实施例1和5的检测峰面积均保持较高水平，且随着浸提时间增加，检测峰面积增加不明显。From Examples 1, 5 and Comparative Example 4, it can be seen that when the extraction time is 2h-3h, the extraction effect is better, and the detection peak areas of Examples 1 and 5 maintain a relatively high level, and increase with the extraction time , the detection peak area did not increase significantly.
由实施例1和6可知，当干燥条件为80℃和1h时，峰面积有下降趋势，判断为过高的温度会使微球破裂，干扰后续的检测分析。From Examples 1 and 6, it can be seen that when the drying condition is 80°C and 1 h, the peak area has a downward trend, and it is judged that the microspheres will be broken if the temperature is too high, which will interfere with the subsequent detection and analysis.
由实施例1、7～8可知，当水相为0.1wt％磷酸水溶液或0.01mol/L的磷酸二氢钠水溶液时，以及有机相为乙腈时，均对检测结果有影响。From Examples 1, 7-8, it can be seen that when the aqueous phase is 0.1wt% phosphoric acid aqueous solution or 0.01mol/L sodium dihydrogen phosphate aqueous solution, and when the organic phase is acetonitrile, the detection results are affected.
由实施例1和对比例5可知，干燥前处理对检测结果影响较大，没有干燥的微球中含有其他试剂会对检测产生干扰。From Example 1 and Comparative Example 5, it can be seen that the pre-drying treatment has a greater impact on the detection results, and the presence of other reagents in the undried microspheres will interfere with the detection.
以上所述仅为本申请的具体实施例而已，并不用于限制本申请，对于本领域的技术人员来说，本申请可以有各种更改和变化。凡在本申请的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本申请的保护范围之内。The above descriptions are only specific embodiments of the present application, and are not intended to limit the present application. For those skilled in the art, various modifications and changes may be made to the present application. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of this application shall be included within the protection scope of this application.
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| GB201315936D0 (en)* | 2013-09-06 | 2013-10-23 | Biocompatibles Uk Ltd | Radiopaque polymers |
| GB201315923D0 (en)* | 2013-09-06 | 2013-10-23 | Biocompatibles Uk Ltd | Radiopaque polymers |
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| GB201315923D0 (en)* | 2013-09-06 | 2013-10-23 | Biocompatibles Uk Ltd | Radiopaque polymers |
| US20190192438A1 (en)* | 2017-12-22 | 2019-06-27 | Shandong Rientech Medical Technology Co.,Ltd | Method for preparing degradable drug-loaded microsphere for embolization, and product obtained therefrom |
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