WO2024060426A1 - 一种测定马来酸甲麦角片剂中乙醇量的方法 - Google Patents

一种测定马来酸甲麦角片剂中乙醇量的方法 Download PDF

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WO2024060426A1
WO2024060426A1 PCT/CN2022/138255 CN2022138255W WO2024060426A1 WO 2024060426 A1 WO2024060426 A1 WO 2024060426A1 CN 2022138255 W CN2022138255 W CN 2022138255W WO 2024060426 A1 WO2024060426 A1 WO 2024060426A1
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ethanol
solution
measuring
minutes
methylergot
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PCT/CN2022/138255
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French (fr)
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高燕霞
韩彬
李挥
徐艳梅
闫凯
许峰
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河北省药品医疗器械检验研究院(河北省化妆品检验研究中心)
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/30Control of physical parameters of the fluid carrier of temperature
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/32Control of physical parameters of the fluid carrier of pressure or speed
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/64Electrical detectors
    • G01N30/68Flame ionisation detectors
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/30Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3007Control of physical parameters of the fluid carrier of temperature same temperature for whole column
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/32Control of physical parameters of the fluid carrier of pressure or speed
    • G01N2030/324Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate

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  • the invention belongs to the field of drug analysis and detection, and is specifically a method for measuring the amount of ethanol in methylergot maleate tablets.
  • Methysergometrine maleate is internationally recognized as the first choice drug for the treatment of postpartum hemorrhage. There is no self-developed product of this variety on the market in China.
  • ethanol is the tableting step, and the wet method is used to prepare methysergonovine maleate tablets.
  • the wetting agent used in the tablets in theory, the ethanol should be completely removed in the subsequent drying step. Therefore, if there is residual ethanol in the methysergometrine maleate tablets that exceeds the national standard limit, it indicates that the process parameter settings are unreasonable. , further adjustments and improvements are needed, but there is currently no method for determining the amount of ethanol in methylergot maleate tablets.
  • the purpose of the present invention is to provide a method for measuring the amount of ethanol in methylergot maleate tablets in view of the above problems, which includes the following steps:
  • the chromatographic conditions are:
  • Programmed temperature rise the initial column temperature is 40°C, maintained for 5 minutes, heated to 120°C at a rate of 10°C per minute, maintained for 1 minute, and then heated to 240°C at a rate of 30°C per minute, maintained for 2 minutes.
  • Inlet temperature 250°C;
  • Carrier gas high purity nitrogen, flow rate: 3.0ml/min;
  • the blank solution is ultrapure water.
  • the reference solution is prepared by: accurately weighing 50 mg of the ethanol reference solution, placing it in a 100 ml measuring bottle, diluting to the mark with water, shaking well, accurately measuring 2 ml and placing it in a headspace bottle, and sealing with a cap.
  • the preparation of the test solution take 20 tablets of this product, grind it finely, take 0.2g, weigh it accurately, put it in a 20ml headspace bottle, add 2ml of water accurately, seal it with a cap, and shake it gently. Shake for 10 minutes.
  • the present invention adopts gas chromatography-headspace sampling method, based on external standard method and calculated by peak area, to determine the residual ethanol content in methysergonovine maleate tablets.
  • the method is fast, efficient, and low-toxic, which is of great significance to ensuring the safety of people's medication. It also has short analysis time and low inspection cost. No more toxic and harmful reagents are used in the method, which is in line with the development trend of green industrialization in my country's pharmaceutical industry.
  • Figure 1 shows a typical diagram of system suitability
  • Figure 2 is the chromatogram of the blank solution
  • Figure 3 is the chromatogram of the reference solution
  • Figure 4 is the solution chromatogram of the test product (batch number: 200926);
  • Figure 5 is the solution chromatogram of the test product (batch number: 201002);
  • Figure 6 is the solution chromatogram of the test product (batch number: 201104).
  • German Mettler XS205 electronic analytical balance German Mettler XS205 electronic analytical balance.
  • Test product Methysergide maleate tablets, homemade in the laboratory,
  • Programmed temperature rise the initial column temperature is 40°C, maintained for 5 minutes, heated to 120°C at a rate of 10°C per minute, maintained for 1 minute, and then heated to 240°C at a rate of 30°C per minute, maintained for 2 minutes.
  • Inlet temperature 250°C;
  • Carrier gas high purity nitrogen, flow rate: 3.0ml/min;
  • Preparation of reference substance solution Precisely weigh 50 mg of the ethanol reference substance and place it in a 100 ml measuring bottle, dilute it with water to the mark, shake well, accurately measure 2 ml and place it in a headspace bottle, and seal it with a gland.
  • test solution Take 20 tablets of this product, grind it finely, weigh 0.2g accurately, place it in a 20ml headspace bottle, add 2ml of water accurately, seal with a cap, and shake gently for 10 minutes.
  • Preparation of system suitability solution Take headspace injection of reference solution, and the separation between the main peak and adjacent impurity peaks should be greater than 1.5.
  • the quantitative limit concentration of ethanol is: 15 ⁇ g/ml
  • the detection limit concentration is: 5 ⁇ g/ml.
  • the peak area (A) is used to perform linear regression processing on the corresponding concentration (C).
  • the results show that there is a good linear relationship between ethanol concentration and peak area in the concentration range of 5 ⁇ g/ml to 1.0 mg/ml.
  • the method of the present invention is fast, efficient, and low-toxic.
  • Three batches of sample data show that after adjusting and improving the process parameters, the residual amount of ethanol in the finished product can be effectively reduced, which is of great significance in ensuring the safety of people's medication, and the analysis time is short.
  • the test cost is low, and no more toxic and harmful reagents are used in the method, which is in line with the development trend of green industrialization in my country's pharmaceutical industry.

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Abstract

本发明涉及药物分析检测领域,提供了一种测定马来酸甲麦角片剂中乙醇量的方法。本发明包括如下步骤:分别将空白溶液、对照品溶液和供试品溶液加注入到气相色谱仪中,记录色谱图,按外标法以峰面积计算马来酸甲麦角片剂中残留的乙醇的含量。本发明方法快捷、高效、低毒,对指导企业调整工艺参数、保障人民用药安全有重要意义,且分析时间短,检验成本低,方法中没有使用更多有毒有害试剂,符合我国制药行业绿色产业化发展趋势。

Description

一种测定马来酸甲麦角片剂中乙醇量的方法 技术领域
本发明属于药物分析检测领域,具体是一种测定马来酸甲麦角片剂中乙醇量的方法。
背景技术
马来酸甲麦角新碱是国际公认治疗产后出血首选药,该品种国内尚无自研产品上市,在马来酸甲麦角新碱片剂中制备的工艺中,乙醇是压片步骤,湿法制粒采用的润湿剂,在后续烘干步骤,理论上乙醇应完全除尽,因此马来酸甲麦角新碱片剂中如果有超出国家标准限度的残留的乙醇,指征工艺参数设置不合理,需进一步调整、改进,但目前还没有一种测定马来酸甲麦角片剂中乙醇量的方法。
发明内容
本发明的目的是针对以上问题,提供了一种测定马来酸甲麦角片剂中乙醇量的方法,包括以下步骤:
分别将空白溶液、对照品溶液和供试品溶液加注入到气相色谱仪中,记录色谱图,按外标法以峰面积计算马来酸甲麦角片剂中乙醇的含量;
色谱条件为:
色谱柱:Agilent DB-624(0.53mm×30m,3μm);
程序升温:起始柱温为40℃,维持5分钟,以每分钟10℃的速率升温至120℃,维持1分钟,再以每分钟30℃的速率升温至240℃,维持2分钟。
进样口温度:250℃;
检测器温度:280℃;
载气:高纯氮气,流速:3.0ml/min;
顶空瓶平衡温度:80℃,平衡时间:30分钟。
优选的,所述空白溶液为超纯水。
优选的,所述对照品溶液的制备:精密称取乙醇对照品50mg,置100ml量瓶中,用水稀释至刻度,摇匀,精密量取2ml置顶空瓶中,压盖密封。
优选的,其特征在于,供试品溶液的制备:取本品20片,研细,取0.2g,精密称定,置20ml顶空瓶中,准确加入水2ml,压盖密封,轻轻振摇10分钟。
与现有技术相比,本发明的有益效果如下:
本发明采用气相色谱-顶空进样法,按外标法,以峰面积计算,测定马来酸甲麦角新碱片剂中残留的乙醇含量。方法快捷、高效、低毒,对保障人民用药安全有重要意义,且分析时间短,检验成本低,方法中没有使用更多有毒有害试剂,符合我国制药行业绿色产业化发展趋势。
附图说明
图1为系统适用性典型图谱;
图2为空白溶液色谱图;
图3为对照品溶液色谱图;
图4为供试品(批号:200926)溶液色谱图;
图5为供试品(批号:201002)溶液色谱图;
图6为供试品(批号:201104)溶液色谱图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
1、仪器与试药
仪器:安捷伦7890B气相色谱仪;
氢火焰离子化检测器(FID);
纯水氢气发生器(电阻率18.2Ω);
SGK-2LB低噪空气泵(北京东方精华苑科技有限公司);
Open LBACDS Chem Station Edition工作站;
德国梅特勒XS205电子分析天平。
试剂:超纯水为实验室自制。
对照品:乙醇,来源:中国食品药品检定研究院,批号:130106-202105,含量:100.0%
供试品:马来酸甲麦角新碱片,实验室自制,
批号:200926、201024、201122。
2、方法
2.1色谱条件
色谱柱:Agilent DB-624(0.53mm×30m,3μm);
程序升温:起始柱温为40℃,维持5分钟,以每分钟10℃的速率升温至120℃,维持1分钟,再以每分钟30℃的速率升温至240℃,维持2分钟。
进样口温度:250℃;
检测器温度:280℃;
载气:高纯氮气,流速:3.0ml/min;
顶空瓶平衡温度:80℃,平衡时间:30分钟。
2.2溶液的配制
空白溶液的配制:超纯超纯水;
对照品溶液的配制:精密称取乙醇对照品50mg置100ml量瓶中,用水稀释至刻度,摇匀,精密量取2ml置顶空瓶中,压盖密封。
供试品溶液的配制:取本品20片,研细,取0.2g,精密称定,置20ml顶空瓶中,准确加水2ml,压盖密封,轻轻振摇10分钟。
系统适用性溶液的配制:取对照品溶液顶空进样,主峰与相邻杂质峰之间分离度应大于1.5。
3、方法学验证
3.1专属性实验
取系统适用性溶液、空白溶液、对照品溶液和供试品溶液各分别注入气相色谱仪,记录色谱图,结果如图1-图6所示。
结果表明,在该色谱条件下,溶剂不干扰样品测定,乙醇峰与前后杂质峰均能达到基线分离。
3.2定量限和检出限
精密量取对照品溶液,逐级稀释,注入气相色谱仪,记录色谱图,至信噪比S/N约为10,即为定量限;
精密量取对照品溶液,逐级稀释,注入气相色谱仪,记录色谱图,至信噪比S/N约为3,即为检出限。
该色谱条件下,乙醇定量限浓度为:15μg/ml,检出限浓度为:5μg/ml。
3.3线性及范围
精密称取乙醇对照品0.5011g置100ml量瓶中,加水稀释至刻度,摇匀,作为对照品贮备液,精密量取0.1ml、1ml、5ml、10ml、20ml、30ml分置100ml量瓶中,加水稀释至刻度,摇匀,制得标准溶液(1)、(2)、(3)、(4)、(5),浓度分别为5μg/ml、50μg/ml、0.25mg/ml、0.5mg/ml、1.0mg/ml。按上述色谱条件进样测定,记录峰面积。以峰面积(A)对对应浓度(C)进行线性回归处理,线性方程为A=2590C-1.489,相关系数r=0.9998。结果表明:乙醇在5μg/ml~1.0mg/ml浓度范围内,浓度与峰面积呈良好的线性关系。
3.4准确度
取供试品1批(批号:201104),精密称取0.2g,平行9份,置顶空瓶中, 分别加入上述标准溶液(3)、(4)、(5)各2ml,密封,轻轻振摇10分钟,依法测定,记录色谱图,按外标法计算。平均回收率为99.7%,RSD为1.2%,见表1。
Figure PCTCN2022138255-appb-000001
3.5精密度
3.5.1重复性
取对照品溶液6份,连续进样,乙醇峰面积的相对标准偏差为0.55%
3.5.2中间精密度
取供试品1批。批号:200926,照上述方法配制6份供试品溶液,注入气相色谱仪,测定结果,乙醇的平均含量为0.26%,RSD为0.7%;
3.6稳定性
取供试品溶液和对照品溶液,室温放置,分别在0h、2h、4h、6h、8h注入气相色谱仪,记录乙醇峰面积,RSD分别为1.8%和0.6%,溶液状态下,供试品和对照品在8小时之内稳定性良好。
4、样品测定
取实验室自制样品3批,批号:200926、201024、201122,按拟定方法进样测定,结果见表2。
样品测定结果(%)
Figure PCTCN2022138255-appb-000002
综上所述,本发明的方法快捷、高效、低毒,三批样品数据显示,调整、改进工艺参数后,可以有效降低成品中乙醇残留量,保障人民用药安全有重要意义,且分析时间短、检验成本低、方法中没有使用更多有毒有害试剂,符合我国制药行业绿色产业化发展趋势。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。

Claims (4)

  1. 一种测定马来酸甲麦角片剂中乙醇量的方法,其特征在于,包括以下步骤:
    分别将空白溶液、对照品溶液和供试品溶液加注入到气相色谱仪中,记录色谱图,按外标法以峰面积计算马来酸甲麦角片剂中乙醇的含量;
    色谱条件为:
    色谱柱:Agilent RESTEK Bef 0.32mm×30m,0.25μm;
    程序升温:起始柱温为40℃,维持5分钟,以每分钟10℃的速率升温至150℃,维持2分钟,再以每分钟20℃的速率升温至200℃,维持2分钟;
    进样口温度:220℃;
    检测器温度:250℃;
    载气:高纯氮气,流速:3.0ml/min;
    顶空瓶平衡温度:80℃,平衡时间:30分钟。
  2. 根据权利要求1所述的一种测定马来酸甲麦角片剂中乙醇量的方法,其特征在于,所述空白溶液为超纯水。
  3. 根据权利要求1所述的一种测定马来酸甲麦角片剂中乙醇量的方法,其特征在于,所述对照品溶液的制备:称取乙醇50mg置100ml量瓶中,用水稀释至刻度,摇匀,量取2ml置顶空瓶中,压盖密封。
  4. 根据权利要求1所述的一种测定马来酸甲麦角片剂中乙醇量的方法,其特征在于,供试品溶液的制备:取本品20片,研细,取0.2g,称定,置20ml顶空瓶中,准确加入水2ml,压盖密封,震荡10分钟。
PCT/CN2022/138255 2022-09-22 2022-12-10 一种测定马来酸甲麦角片剂中乙醇量的方法 WO2024060426A1 (zh)

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