CN111896653A - 一种保健品中非法添加盐酸丁福明的检测方法 - Google Patents
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Abstract
本发明公开了一种保健品中非法添加盐酸丁福明的检测方法,具体是涉及一种降糖类保健品胶囊中盐酸丁福明的检测方法。本方法以甲醇溶液超声提取样品,利用超高效液相色谱‑三重四级杆串联质谱法检测。主要具体步骤为:标准溶液配制,甲醇提取降糖类保健品胶囊中目标物,超高效液相色谱‑质谱联用仪检测,外标法定量。本发明利用甲醇溶液提取,UPLC‑MS/MS法进行检测,该方法回收率、重复性、灵敏度和检测限均满足于国标要求。本发明具有快捷,简便,高效等特点。
Description
技术领域
本发明涉及一种保健品中非法添加化学药物的检测方法,具体是涉及一种降糖胶囊中盐酸丁福明的含量检测方法。
背景技术
随着我国老年化人口的不断加剧,我国众多数量的糖尿病、糖耐量异常人群,降糖药物及相关保健品需求逐渐增多。现代医学研究表明,糖尿病患者与糖耐量人群对高糖食品摄入致使机体代谢紊乱,进而产生多种并发症,如心血管、肾脏、神经系统、肥胖等急性、慢性疾病,同时具有较高的病死率风险。糖尿病给人们的健康带来巨大的隐患,已成为我国乃至全世界各国人们高发的病理学疾病之一,对各国公共卫生体系造成严重的负担。因此,各国致力于针对糖尿病患者的治疗药物研发及生产,而降糖类保健品的开发也备受生产企业及患者青睐,同时也为不法分子的渗入提供了条件。
近年来,降糖类药品和保健品中非法添加降糖化学成分的报道屡见不鲜,此类非法添加行为对患者的治疗带来严重的安全隐患,对糖尿病患者健康造成严重的危害。为此,国家及省市对非法添加化学药物的监督管理和各种严打专项整治活动正有序开展,并取得了显著成效。因此,建立一种高通量的降糖保健品中非法添加化学药物的检测方法,为防止制假行为尤为重要。盐酸丁福明又称盐酸丁二胍,化学名称为:1-丁基二胍。属于二胍类化学降糖药物中的一种,由于存在严重的乳酸中毒不良反应,目前已被我国包括大多数国家列为禁药淘汰,在国外有少数国家上市,但我国尚未获批准。
本发明公开了一种检测降糖保健品胶囊中丁福明的方法,包括以下步骤:1)样品溶液的制备:利用甲醇溶液提取,得到样品溶液;2)配制丁福明标准溶液:用丁福明标准品和甲醇配制系列标准溶液;3)样品检测:将样品储备液与丁福明标准溶液分别注入到超高效液相色谱-质谱联用仪,通过标准曲线,利用外标法检测样品中的丁福明含量。该方法具有灵敏度高、回收率好,快捷,简便,高效等特点,可用于同类保健品胶囊和颗粒剂保健食品中非法添加丁福明含量的高通量分析。
发明内容
本发明的目的在于利用高通量检测,提供一种降糖保健品中非法添加丁福明的含量检测方法。本发明在现有报道的检测方法(包括HPLC-MS-MS等)基础上,采用更为快捷、简便、高效的超高效液相色谱-质谱联用仪对保健品中丁福明含量的测定,其具有灵敏度高、回收率好,快捷,简便,高效等特点,对快速测定保健品中丁福明的检测具有实际应用和指导意义。
本发明的技术方案如下:
一种保健品中非法添加化合物盐酸丁福明的检测方法,包括以下步骤,S1、标准溶液配制:配制成1.0mg·mL-1的标准储备液,将所述标准储备液用50%的甲醇溶液逐级稀释配制成系列标准浓度,分别为:100μg·mL-1,50μg·mL-1,25μg·mL-1,10μg·mL-1,5μg·mL-1,1μg·mL-1,建立标准曲线,计算线性方程及相关系数(r值大于0.99)。S2、样品前处理:取糖胶囊样品的胶囊去壳,将内容物研磨成细粉,精密称取0.5g,置于100mL容量瓶中,加入70mL 50%甲醇的溶液,超声提取,放至室温,加入50%甲醇溶液至刻度线,混匀后过滤,备用液。使用时混匀过滤,调整稀释倍数确保供试样品溶液的浓度在标准曲线线性范围内。
S3、检测:分别取一定量步骤S1中的系列标准溶液及步骤S2中的备用液,注入UPLC-MS/MS仪中,通过标准品溶液浓度及检测峰面积,依据S1中的标准工作曲线,并对S2备用液含量进行测定。
优选的,步骤S1所配制的标准系列浓度分别为100μg·mL-1,50μg·mL-1,25μg·mL-1,10μg·mL-1,5μg·mL-1,1μg·mL-1。
优选的,步骤S1配制标准系列浓度的方法为逐级稀释法。
优选的,步骤S2中所述过滤为采用0.45μm聚四氟乙烯滤膜过滤。
优选的,步骤S2中所述降糖胶囊样品储备液浓度在S1标准曲线线性范围内。
优选的,步骤S3中所述检测仪器为超高效液相色谱-质谱联用仪(即UPLC-MS/MS)的测试条件为:
(1)超高效液相色谱条件
色谱仪:Agilent 1290高效液相色谱仪(美国Agilent公司),色谱柱:AgilentEclipse plus C-18柱(1.8μm,2.1mm×50mm);流速:0.3mL·min-1;柱温:40℃;进样量:5μL;流动相A:0.2%甲醇水溶液,流动相B:乙腈-甲醇溶液(6:4);梯度洗脱程序:0~2.0min,80%A,20%B;2.1~3.0min,60%~40%A,40%~60%B;3.1~4.0min,40%~30%A,60%~70%B;4.1~6.0min,30%~20%A,70%~80%B;6.1~10.0min,80%A,20%B(见表1所示)。
表1超高效液相色谱梯度洗脱条件
注:A=0.2%甲醇水溶液;B=乙腈-甲醇(6:4)
(2)质谱条件
离子源条件:ESI+正离子扫描;检测方式:多反应监测(MRM);电喷雾电压:500V;干燥气温度:325℃;干燥气流量:8L·min-1;鞘气温度:370℃;鞘气流量:10L·min-1;毛细管电压:4000V。
根据权利要求4所述的检测方法,其特征在于:所述流动相A和流动相B的体积比6:4组成混合物;所述质谱条件中质谱扫描信息为:定量离子对为158.0/60.1,碰撞能为28.0V,源内碎裂电压250V。
本发明的有益效果是:
(1)在盐酸丁福明流动相的选择中,发明人经过大量的试验,发现采用乙腈-甲醇(6:4)的体系,目标物的峰形较好,响应较高。
(2)发明人采用0.45μm聚四氟乙烯(PTFE)滤膜过滤对标准品及样品储备液过滤,能有效去除颗粒物杂质,对检测目标影响较小。
(3)发明人对检测方法的方法学进行考察,包括精密度、重复性、稳定性和加标回收率等,表明该方法具有较高的使用性。
1)精密度:精密吸取5μL浓度为10μg·mL-1标准溶液6次,按S3步骤进样,测定峰面积,计算出丁福明的RSD值为2.5%。
2)重复性考察:吸取同一批次测试样品,制备成供试样品溶液6份,按S3步骤进样,测定峰面积,计算6次盐酸丁福明的RSD值为3.8%。
3)稳定性试验:精密吸取同一份供试样品溶液10μL,分别于0h、2h、4h、6h、8h、10h、12h后按S3进样,测定峰面积,计算7次不同放置时间内的RSD值为4.8%,表明在室温放置12小时内样品较为稳定。
4)加样回收率试验:精密称取含有丁福明化合物的胶囊粉末0.5g,按S2步骤制备,并将其分为3组,分别低、中、高3种浓度的标准溶液(即0.2μg·g-1、5μg·g-1、10μg·g-1),按S3步骤进行测定,计算3种浓度的回收率的RSD值为7.79%(见表2所示)。
表2加样回收率
说明附图
图1为本发明采用外标法定量,所得到标准曲线的回归方程、相关系数及线性范围。
图2为盐酸丁福明浓度为1μg·mL-1下的信噪比。
图3为实施例的空白样品和加标样品测试结果,图中黑色代表空白样品图谱,红色代表加标前样品图谱,蓝色代表加标后样品图谱。
具体实施方式
以下通过具体实施方式对本发明的技术方案进行进一步的说明和描述。
实施方式
一、仪器、试剂和材料
盐酸丁福明(盐酸丁二胍)标准品(纯度≥98%,购自日本)
甲醇、乙腈(色谱纯,德国Sigma公司)
超纯水(电阻率≥18.2MΩ·cm,美国Millipore公司)
Agilent 1290高效液相色谱仪(美国Agilent公司);Agilent G6460三重四级杆质谱仪,配有电喷雾离子源(ESI,美国Agilent公司);分析天平(瑞士梅特勒;型号:AB204-S;感量0.1mg);涡旋混匀器(江苏其林贝尔公司);离心机(Sigma-Aldrich公司);0.45μm聚四氟乙烯(PTFE)针头式过滤器(天津津腾实验设备有限公司)。
二、检测过程
(1)标准溶液配制:配制成1.0mg.mL-1的标准储备液,将所述标准储备液用50%的甲醇溶液逐级稀释配制成系列标准浓度,分别为:100μg·mL-1,50μg·mL-1,25μg·mL-1,10μg·mL-1,5μg·mL-1,1μg·mL-1,建立标准曲线,计算线性方程及相关系数(r值大于0.99)。(2)样品前处理:取糖胶囊样品的胶囊去壳,将内容物研磨成细粉,精密称取0.5g,置于100mL容量瓶中,加入70mL 50%甲醇的溶液,超声提取,放至室温,加入50%甲醇溶液至刻度线,混匀后过滤,备用液。使用时混匀过滤,调整稀释倍数确保供试样品溶液的浓度在标准曲线线性范围内。
(3)检测:分别取一定量步骤S1中的系列标准溶液及步骤S2中的备用液,注入UPLC-MS/MS仪中,通过标准品溶液浓度及检测峰面积,依据S1中的标准工作曲线,并对S2备用液含量进行测定。所述的三重四级杆串联质谱仪的测试条件为:
(1)超高效液相色谱条件
色谱柱:Agilent Eclipse plus C-18柱(1.8μm,2.1mm×50mm);流速:0.3mL.min-1;柱温:40℃;进样量:5μL;流动相A:0.2%甲醇水溶液,流动相B:乙腈-甲醇溶液(6:4);梯度洗脱程序:0~2.0min,80%A,20%B;2.1~3.0min,60%~40%A,40%~60%B;3.1~4.0min,40%~30%A,60%~70%B;4.1~6.0min,30%~20%A,70%~80%B;6.1~10.0min,80%A,20%B(见表1所示)。
表1超高效液相色谱梯度洗脱条件
注:A=0.2%甲醇水溶液;B=乙腈-甲醇(6:4)
(2)质谱条件
离子源条件:ESI+正离子扫描;检测方式:多反应监测(MRM);电喷雾电压:500V;干燥气温度:325℃;干燥气流量:8L·min-1;鞘气温度:370℃;鞘气流量:10L·min-1;毛细管电压:4000V。
图1为本发明采用外标法定量,所得到标准曲线的回归方程、相关系数及线性范围。
图2为盐酸丁福明浓度为1μg·mL-1下的信噪比。
图3为实施例的空白样品和加标样品测试结果,图中黑色代表空白样品图谱,红色代表加标前样品图谱,蓝色代表加标后样品图谱。
以10倍信噪比时相应浓度确定检测低限,见表3;本发明对盐酸丁福明的仪器检测限为0.018μg·g-1;在10倍稀释条件下的盐酸丁福明方法检测限为0.18μg·g-1,说明本方法灵敏度高。
表3检测低限与定量限
实施例
以市售某降糖保健品胶囊为测试对象,分别对方法学进行了考察,具体方法如下:
(1)精密度:精密吸取5μL 10μg·mL-1标准溶液6次,按S3步骤进样,测定峰面积,计算出丁福明的RSD值为2.5%。
(2)重复性考察:吸取同一批次测试样品,制备成供试样品溶液6份,按S3步骤进样,测定峰面积,计算6次丁福明的RSD值为3.8%。
(3)稳定性试验:精密吸取同一份供试样品溶液10μL,分别于0h、2h、4h、6h、8h、10h、12h后按S3进样,测定峰面积,计算7次不同放置时间内的RSD值为4.8%,表明在室温放置12小时内样品较为稳定。
(4)加样回收率试验:精密称取含有丁福明化合物的胶囊粉末0.5g,按S2步骤制备,并将其分为3组,分别低、中、高3种浓度的标准溶液(即0.2、5、10μg·g-1),按S3步骤进行测定,计算3种浓度的回收率的RSD值为7.79%(见表2所示)。
表2加样回收率
以上测试方法满足药物残留检测的分析要求。
应用本方法对市售的某品牌降糖保健品胶囊中盐酸丁福明含量进行测定,每份样品平行测定两次,结果见表4。
表4市售某品牌中三种降糖保健品胶囊中盐酸丁福明检测结果
以上所述,显示和描述了本发明的基本原理、主要特征和优点。本领域技术人员应该了解本发明不受上述实施例的限制,上述实施例仅为本发明的实施例而已,不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。本发明要求保护范围由所附的权利要求书及其等同物界定。
Claims (5)
1.一种保健品中非法添加化合物盐酸丁福明的检测方法,其特征在于:包括以下步骤,
S1、标准溶液配制:配制成1.0mg·mL-1的盐酸丁福明标准储备液,将所述标准储备液用50%的甲醇溶液逐级稀释配制成系列标准浓度,分别为:100μg·mL-1,50μg·mL-1,25μg·mL-1,10μg·mL-1,5μg·mL-1,1μg·mL-1,建立标准曲线。
S2、样品前处理:取糖胶囊样品的胶囊去壳,将内容物研磨成细粉,精密称取置于容量瓶中,加入50%甲醇溶液,超声提取,放至室温,用50%甲醇补足至刻度,备用液。使用时混匀过滤,调整稀释倍数确保供试样品溶液的浓度在标准曲线线性范围内。
S3、检测:分别取一定量步骤S1中的系列标准溶液及步骤S2中的备用液,注入UPLC-MS/MS仪中,通过标准品溶液浓度及检测峰面积,依据S1中的标准工作曲线,并对S2备用液含量进行测定。
2.根据权利要求1所述的检测方法,其特征在于:步骤S1配制标准系列浓度的方法为逐级稀释法。
3.根据权利要求1所述的检测方法,其特征在于:步骤S2中所述过滤为采用0.45μm聚四氟乙烯滤膜过滤。
4.根据权利要求1所述的检测方法,其特征在于:步骤S3中所述检测仪器为UPLC-MS/MS仪的测试条件为:
(1)超高效液相色谱条件
色谱仪:Agilent 1290高效液相色谱仪(美国Agilent公司),色谱柱:Agilent Eclipseplus C-18柱(1.8μm,2.1mm×50mm);流速:0.3mL·min-1;柱温:40℃;进样量:5μL;流动相A:0.2%甲醇水溶液,流动相B:乙腈-甲醇溶液体积比为6:4;梯度洗脱程序:0~2.0min,80%A,20%B;2.1~3.0min,60%~40%A,40%~60%B;3.1~4.0min,40%~30%A,60%~70%B;4.1~6.0min,30%~20%A,70%~80%B;6.1~10.0min,80%A,20%B。
(2)质谱条件
离子源条件:ESI+正离子扫描;检测方式:多反应监测(MRM);电喷雾电压:500V;干燥气温度:325℃;干燥气流量:8L·min-1;鞘气温度:370℃;鞘气流量:10L·min-1;毛细管电压:4000V。
5.根据权利要求4所述的检测方法,其特征在于:所述流动相A和流动相B的体积比6:4组成混合物;所述质谱条件中质谱扫描信息为:定量离子对为158.0/60.1,碰撞能为28.0V,源内碎裂电压250V。
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