CN107037174A - 山楂中安赛蜜的残留量的测定方法 - Google Patents
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Abstract
本发明提供了一种山楂中安赛蜜的残留量的测定方法,其包括以下步骤:配制安赛蜜标准溶液和绘制标准曲线;采用经过打浆处理制得的山楂浆和烘干山楂核制得的山楂核粉混合进行超声萃取和离心分离,从而制得山楂样品溶液;采用液相色谱‑质谱法检测所述山楂样品溶液,并将所述山楂样品溶液的测定结果与所述标准溶液曲线进行比对,得到所述山楂样品溶液中的安赛蜜含量。本发明提供的上述测定方法通过打浆处理鲜山楂等工艺,可以使得山楂样品溶液中的各组分含量更加接近鲜山楂中对应组分的真实含量,从而提高检测结果的准确度,能够更加准确判断山楂是否经过安赛蜜处理。
Description
技术领域
本发明属于食品检测领域,具体地涉及一种山楂中安赛蜜的残留量的测定方法。
背景技术
安赛蜜是一种食品添加剂,是化学品,类似于糖精,易溶于水,增加食品甜味的,没有营养,口感好,无热量,具有在人体内不代谢、不吸收(是中老年人、肥胖病人、糖尿病患者理想的甜味剂),对热和酸稳定性好等特点,是当前世界上第四代合成甜味剂。它和其它甜味剂混合使用能产生很强的协同效应,一般浓度下可增加甜度30%~50%。安赛蜜具有强烈甜味,甜度约为蔗糖的130倍,呈味性质与糖精相似。高浓度时有苦味。有研究表明,食用安赛蜜过量会对人体的肝脏和神经系统造成危害,特别是对老人、孕妇、小孩危害更为严重。如果短时间内大量食用,会引起血小板减少导致急性大出血。因此部分国家已经禁止使用该种添加剂。我国虽然未禁止此类添加剂的使用,但在国家标准GB 2760中明确规定安赛蜜在各类食品中的最大添加限量,并禁止在鲜水果中使用。
山楂,核果类水果,核质硬,果肉薄,味微酸涩,是中国特有的药果兼用树种,具有降血脂、血压、强心、抗心律不齐等作用;同时山楂含山楂酸等多种有机酸,并含解脂酶,入胃后,能增强酶的作用,促进肉食消化,有助于胆固醇转化,所以,山楂也是健脾开胃、消食化滞、利胆汁、促进胃液分泌、活血化痰的良药,对胸膈脾满、疝气、血淤、闭经等症有很好的疗效。山楂所含的黄酮类和维生素C、胡萝卜素等物质能阻断并减少自由基的生成,能增强机体的免疫力,有防衰老、抗癌的作用山楂中有平喘化痰、抑制细菌、治疗腹痛腹泻的成分。因此,山楂深受人们的喜爱,随着人们对健康越来越重视,对山楂是否经过安赛蜜处理的问题产生了质疑。
发明内容
有鉴于此,确有必要提供一种山楂中安赛蜜的残留量的测定方法,以解决上述问题。
一种山楂中安赛蜜的残留量的测定方法,其包括以下步骤:
配制安赛蜜标准溶液,绘制安赛蜜标准溶液曲线;
将10~15 g鲜山楂清洗干净后去核,得到无核山楂和山楂核;对所述无核山楂进行打浆处理,得到山楂浆;将所述山楂核干燥后破碎研磨成粉,获得山楂核粉;
将所述山楂浆和所述山楂核粉混合置于50mL离心管中,并加入10mL纯净水;然后,先超声提取15~18 min,在以1×104~2×104 r/min的转速离心分离8~10 min,获得首次上清液和首次沉淀物,并收集全部所述首次上清液;向所述首次沉淀物中加入10mL纯净水并超声提取8~12 min,再离心分离5~7 min,收集全部二次上清液;将该二次上清液与所述首次上清液均匀混合,得到山楂上清液;将所述山楂上清液过0.22μm膜,得到山楂样品溶液;
采用液相色谱-质谱法检测所述山楂样品溶液,并将所述山楂样品溶液的测定结果与所述标准溶液曲线进行比对,得到所述山楂样品溶液中的安赛蜜含量。
其中,所述液相色谱-质谱法的检测条件为:所用色谱柱采用:反相C18色谱柱、直径2.1 mm、柱长50 mm、填料粒径1.7 μm;流动相:乙腈- 0.02 mol/L乙酸铵溶液(10/90,υ/υ);流速:0.25 mL/min;柱温: 40℃;进样量:10 μL;液相色谱分析时间不超过3 min;质谱离子源:ESI;扫描方式:负离子模式;毛细管电压:3.0 kV;离子源温度:110℃;脱溶剂气温度:350℃;脱溶剂气流量:600 L/h;锥孔反吹气流量:50 L/h;锥孔电压:28 V。
基于上述,绘制所述安赛蜜标准溶液曲线的方法为:首先,量取浓度为1mg/ml 的安赛蜜原液200 μL,并转移至100ml 的容量瓶中,用纯净水定容,配制成浓度为2 μg/mL的安赛蜜标准储备液;其次,分别量取所述安赛蜜标准储备液0.5 mL、1 mL、2.5 mL、5 mL、15mL、30 mL并转移至六个100mL的容量瓶中,再分别用纯净水定容,配制成浓度分别为10 μg/L、20 μg/L、50μg/L、100 μg/L、300μg/L、600μg/L的安赛蜜标准溶液系列;然后,采用色谱-串联质谱检测器对上述六个安赛蜜标准溶液系列进行检测,得到安赛蜜标准溶液的六次平行测量结果;最后,以上述六次平行测量结果中的目标峰的峰面积为纵坐标(y),安赛蜜标准溶液系列的浓度为横坐标(x),建立标准曲线。
在本发明提供的山楂中安赛蜜的残留量的测定方法中,在对无核山楂进行打浆处理的过程中,山楂中的纤维受到剪切、揉搓及梳理等作用,并产生细纤维化团聚,而山楂中的安赛蜜及其他成分则由于受到机械外力而被挤出来,并部分吸附在纤维上,形成所述山楂浆;在所述山楂浆加入山楂核粉,由于山楂核粉具有粗糙的摩擦面和较大的硬度,在超声萃取过程中可以增强因超声波辐射压强而产生的机械振动幅度、扰动效应强度、击碎强度和搅拌作用等,增大物质分子运动频率和速度,增加溶剂穿透力,从而山楂中的营养成分更加容易进入纯净水中,达到加快萃取速度、缩短萃取时间、提高萃取效果的目的。另外,由于山楂经过打浆处理,其中的纤维比较难于进入山楂样品溶液中,而且也有利于帮助离心分离产物上清液和沉淀物分离,使得山楂样品溶液中的各组分含量更加接近鲜山楂中对应组分的真实含量,从而提高检测结果的准确度,能够更加准确判断山楂是否经过安赛蜜处理。
具体实施方式
图1为本发明实施例提供的安赛蜜标准溶液建立的标准曲线图。
图2为本发明实施例提供的安赛蜜标准溶液的色谱图。
图3为本发明实施例提供的山楂样品溶液中的安赛蜜的色谱图。
具体实施方式
下面通过具体实施方式,对本发明的技术方案做进一步的详细描述。
本发明实施例提供一种山楂中安赛蜜的残留量的测定方法,其包括以下步骤:
(一)配制安赛蜜标准溶液,绘制安赛蜜标准溶液曲线;该步骤(一)具体包括以下分步骤:
首先,量取浓度为1mg/ml 的安赛蜜原液200 μL,并转移至100ml 的容量瓶中,用纯净水定容,配制成浓度为2 μg/mL的安赛蜜标准储备液。
其次,分别量取所述安赛蜜标准储备液0.5 mL、1 mL、2.5 mL、5 mL、15 mL、30 mL并转移至六个100mL的容量瓶中,再分别用纯净水定容,配制成浓度分别为10 μg/L、20 μg/L、50μg/L、100 μg/L、300μg/L、600μg/L的安赛蜜标准溶液系列。
然后,采用色谱-串联质谱检测器对上述六个安赛蜜标准溶液系列进行检测,其中,该液相色谱-质谱法的检测条件为:所用色谱柱采用:反相C18色谱柱、直径2.1 mm、柱长50 mm、填料粒径1.7 μm;流动相:乙腈- 0.02 mol/L乙酸铵溶液(10/90,υ/υ);流速:0.25mL/min;柱温: 40℃;进样量:10 μL;液相色谱分析时间不超过3 min;梯度洗脱程序见表1。质谱离子源:ESI;扫描方式:负离子模式;毛细管电压:3.0 kV;离子源温度:110℃;脱溶剂气温度:350℃;脱溶剂气流量:600 L/h;锥孔反吹气流量:50 L/h;锥孔电压:28.0V;母离子(m/z) 162.0;子离子(m/z) 82.10、78.10;对应的碰撞能量为15.0V、15.0V;定量离子(m/z)82.10。
表1 梯度洗脱程序
上述六个安赛蜜标准溶液系列的六次平行测量结果如表2所示。安赛蜜标准溶液的色谱图如图2所示。
表2 安赛蜜标准溶液系列的测量结果
浓度(μg/L) | 10 | 20 | 50 | 100 | 300 | 600 |
峰面积 | 4710 | 8933 | 22109 | 44017 | 132976 | 259911 |
最后,以上述表2中的峰面积为纵坐标(y ),安赛蜜标准溶液系列的浓度为横坐标(x),建立绘制图1所示的标准曲线,得到安赛蜜标准溶液的线性回归方程:y = 433.7x +708.3,相关系数平方0.999,线性范围10~600μg/L,检出限1.0 μg/L。
(二)将11.6 g鲜山楂清洗干净后去核,得到无核山楂和山楂核;对所述无核山楂进行打浆处理,得到山楂浆;将所述山楂核干燥后破碎研磨成粉,获得山楂核粉。
(三)将所述山楂浆和所述山楂核粉混合置于50mL离心管中,并加入10mL纯净水;然后,先超声提取15 min,在以1.5×104 r/min的转速离心分离10 min,获得首次上清液和首次沉淀物,并收集全部所述首次上清液;向所述首次沉淀物中加入10mL纯净水并超声提取8 min,再离心分离7 min,收集全部二次上清液;将该二次上清液与所述首次上清液均匀混合,得到山楂上清液;将所述山楂上清液过0.22μm膜,得到山楂样品溶液。
(四)采用与步骤(一)相同条件的检测条件检测所述山楂样品溶液,所述山楂样品溶液的色谱图如3所示,从图3中可以看出在1.52min处有安赛蜜的特征峰,且所述山楂样品溶液中安赛蜜的峰面积为9903,带入上述安赛蜜标准溶液的线性回归方程中,即可得到山楂样品中的安赛蜜的浓度为21.20 μg/L。由于我国不允许鲜水果中添加安赛蜜,所以本发明实施例提供的鲜山楂的甜味异常,有影响消费者身体健康的隐患。
本发明提供的测定方法的空白加标回收率试验
按照现有的空白加标回收试验方法,制得安赛蜜浓度为50 μg/L、200 μg/L的加标溶液,按照步骤(一)中提供的测定方法进行检测,检测结果为:浓度为50 μg/L的峰面积为23191,计算得出加标回收率为103.7%,相对标准偏差为4%;浓度为200 μg/L的峰面积为89583,计算得出加标回收率为102.5%,相对标准偏差为3%。
最后应当说明的是:以上实施例仅用以说明本发明的技术方案而非对其限制;尽管参照较佳实施例对本发明进行了详细的说明,所属领域的普通技术人员应当理解:依然可以对本发明的具体实施方式进行修改或者对部分技术特征进行等同替换;而不脱离本发明技术方案的精神,其均应涵盖在本发明请求保护的技术方案范围当中。
Claims (2)
1.一种山楂中安赛蜜的残留量的测定方法,其包括以下步骤:
配制安赛蜜标准溶液,绘制安赛蜜标准溶液曲线;
将10~15 g鲜山楂清洗干净后去核,得到无核山楂和山楂核;对所述无核山楂进行打浆处理,得到山楂浆;将所述山楂核干燥后破碎研磨成粉,获得山楂核粉;
将所述山楂浆和所述山楂核粉混合置于50mL离心管中,并加入10mL纯净水;然后,先超声提取15~18 min,在以1×104~2×104 r/min的转速离心分离8~10 min,获得首次上清液和首次沉淀物,并收集全部所述首次上清液;向所述首次沉淀物中加入10mL纯净水并超声提取8~12 min,再离心分离5~7 min,收集全部二次上清液;将该二次上清液与所述首次上清液均匀混合,得到山楂上清液;将所述山楂上清液过0.22μm膜,得到山楂样品溶液;
采用液相色谱-质谱法检测所述山楂样品溶液,并将所述山楂样品溶液的测定结果与所述标准溶液曲线进行比对,得到所述山楂样品溶液中的安赛蜜含量。
2. 根据权利要求1所述的山楂中安赛蜜的残留量的测定方法,其特征在于,绘制所述安赛蜜标准溶液曲线的方法为:首先,量取浓度为1mg/ml 的安赛蜜原液200 μL,并转移至100ml 的容量瓶中,用纯净水定容,配制成浓度为2 μg/mL的安赛蜜标准储备液;其次,分别量取所述安赛蜜标准储备液0.5 mL、1 mL、2.5 mL、5 mL、15 mL、30 mL并转移至六个100mL的容量瓶中,再分别用纯净水定容,配制成浓度分别为10 μg/L、20 μg/L、50μg/L、100 μg/L、300μg/L、600μg/L的安赛蜜标准溶液系列;然后,采用色谱-串联质谱检测器对上述六个安赛蜜标准溶液系列进行检测,得到安赛蜜标准溶液的六次平行测量结果;最后,以上述六次平行测量结果中的目标峰的峰面积为纵坐标(y),安赛蜜标准溶液系列的浓度为横坐标(x),建立标准曲线。
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