CN108051534A - 一种快速筛查中成药和保健品中非法添加的132种化学药物的方法 - Google Patents
一种快速筛查中成药和保健品中非法添加的132种化学药物的方法 Download PDFInfo
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Abstract
本发明公开了一种快速筛查中成药和保健品中非法添加的132种化学药物的方法。本发明方法采用Agilent Poroshell 120 EC‑C18色谱柱进行分离，以0.1％甲酸水‑乙腈作为流动相；采用电喷雾电离正离子模式，采用预设定多反应监测模式。结果表明本发明方法对132种化学药物在线性范围内线性关系良好；定量限在2μg/Kg～200μg/Kg之间；在低、中、高三个添加水平下的回收率为43.36％～114.92％；RSD为0.4％～14.81％。该方法灵敏度高、专属性强、简便快速，可有效用于保健品及中成药样品中132种非法添加化学药物的同时快速筛查。
Description
技术领域
本发明具体涉及一种快速筛查中成药和保健品中非法添加的132种化学药物的方法。
背景技术
随着人们生活水平的提高以及对西药会产生抗药性的警惕，越来越多的人们会选择服用他们认为相对安全的中成药和保健品以维持自身的健康，殊不知不法商家会向中成药和保健品中非法添加各类化学药物，用以在短时间内快速提高药效以牟取最大的非法利益。人们在不知情的情况下，长期服用此类含有非法添加化学药物的中成药和保健品会对人体造成巨大的危害。例如1887年被Morse开发出来的非那西丁，作为市场上第一个解热镇痛药同年在美国上市。因其原形与其代谢物对乙酰氨基酚均有良好的解热镇痛效果，药效强度不亚于阿司匹林，使得非那西丁在临床上被广泛使用。然而在1953年发现，长期服用非那西丁会对人体肾脏造成严重的损害，随后在1970年发现长期服用非那西丁可能会诱发尿道癌，因此在上市的90余年后非那西丁全面退市。一些具有解热镇痛作用的糖皮质激素类药物，消费者长期服用后突然停药，会导致消费者机体糖类、脂肪等代谢紊乱，导致肾上腺功能损害。市面上这些含有非法添加化学药物的中成药和保健品给人民的用药安全带来极大的隐患，严重损害消费者的健康及利益，建立一种全面快速筛查中成药和保健品中非法添加化学药物的方法为目前所需。
发明内容
本发明的目的在于提供一种快速筛查中成药和保健品中非法添加的132种化学药物的方法。
本发明所采取的技术方案是：
一种快速筛查中成药和保健品中非法添加的132种化学药物的方法，包括以下步骤：
一、溶液的配制
对照品溶液的制备：配制132种化学药物的混合标准溶液；
供试品溶液的配制：将待检测的中成药或保健品样品研细混匀，加入甲醇适量，超声处理，冷却，用甲醇定容，滤膜过滤，滤液待上机检测；
二、样品中132种化学药物的定性定量分析
1)将上述混合标准溶液用甲醇配置成个不同浓度混合标准溶液，进行高效液相色谱-串联质谱检测；以被测组分的峰面积为纵坐标，质量浓度为横坐标，进行线性回归，分别制作132种目标化学药物的标准曲线；建立132种化合物的回归方程、相关系数和线性范围；
所述高效液相色谱检测条件为：色谱柱为反相C18液相色谱柱；柱温：30～45℃；流速：0.2～0.4mL/min；进样体积：5～110μL；流动相：A相为0.05～0.2％v/v甲酸水，B相为乙腈，进行梯度洗脱；
所述串联质谱检测条件为：使用电喷雾离子源；采集模式为预设定多反应监测模式；在正离子模式下检测；132种化学药物的质谱参数分别为：
表中*为定量离子；
3)将上述配制好的供试样品溶液进行与混合标准溶液相同的高效液相色谱-串联质谱检测；根据标准曲线分别计算出样品中该132种目标化学药物的含量。
进一步的，所述对照品溶液中的溶剂为甲醇。
进一步的，所述供试品溶液的配制为：将待检测的中成药或保健品1g样品研细混匀，加入甲醇适量，超声处理5～15min，冷却，用甲醇定容至10～40mL，0.22μm滤膜过滤，滤液待上机检测。
进一步的，所述132种化合物的回归方程、相关系数和线性范围情况如下：
表中线性范围的单位是ng/mL，检出限的单位是ng/mL，定量限的单位是ng/mL。
进一步的，所述梯度洗脱的程序为：
其中，A相为0.08～0.12％v/v甲酸水，B相为乙腈。
进一步的，所述高效液相色谱检测条件为：色谱柱为Agilent Pososhell 120EC-C18液相色谱柱；柱温：40℃；流速：0.3mL/min；进样体积：10μL；流动相：A相为0.1％v/v甲酸水，B相为乙腈。
进一步的，串联质谱检测时，离子源温度为500～600℃，喷雾电压：+5.0～+6.0kV。
本发明的有益效果是：
(1)本发明建立了高效液相色谱-质谱联用法检测中成药及保健品中非法添加的132种包括解热镇痛类、降压类、止咳平喘类及抗菌类化学药物的有效分析方法，该方法前处理简单快速，灵敏度高，对保障市场上中成药及保健品的质量安全提供有效的技术手段。
(2)本发明采用甲酸水(0.1％甲酸)-乙腈作为流动相，梯度洗脱模式，电喷雾正离子模式(ESI+)下检测。结果表明，132种化学药物线性关系良好，相关系数均大于0.995，三个添加水平的回收率在43.36％～114.92％之间，定量限在2μg/Kg～200μg/Kg之间。该方法灵敏度高，准确度好，检测通量大，耗时短，适合于中成药和保健品中非法添加化学药物的快速筛查，为打击非法添加及规范中成药和保健品市场，提供技术支持。
具体实施方式
下面结合具体实施例对本发明作进一步的说明。
实施例1一种快速筛查中成药和保健品中非法添加的132种化学药物的方法
1仪器与试药
LC-20AD液相色谱仪，日本SHIMADZU公司；Triple Quad 5500质谱仪，配电喷雾离子(ESI)源，美国SCIEX公司；ST8低温离心机，美国Thermo公司；T10分散机及MS 3Digital涡旋混合器，德国IKA公司；Mili-Q Advantage A10超纯水发生器，美国MILLIPORE公司。
氢化可的松、醋酸去氧皮质酮、氟米龙、地塞米松、泼尼松醋酸酯、醋酸泼尼松龙、倍氯米松、地塞米松醋酸酯、氟替卡松丙酸酯、泼尼松、甲基泼尼松龙、醋酸可的松、氢化可的松醋酸酯、氟米龙醋酸酯、倍他米松戊酸酯、曲安西龙、康力龙、萘啶酸、恶喹酸、西诺沙星、马波沙星、沙氟沙星、双氟沙星、奥比沙星、依诺沙星、磺胺噻唑、磺胺二甲基恶唑、磺胺二甲基异噁唑、磺胺甲噻二唑、磺胺苯酰、磺胺甲氧哒嗪、磺胺氯吡嗪、磺胺苯吡唑、丹诺沙星、磺胺对甲氧嘧啶、磺胺硝苯、磺胺氯哒嗪、磺胺喹恶啉等购自德国Dr.Ehrenstor公司。甲基泼尼松龙醋酸酯、氯倍他松丁酸酯、二氟拉松双醋酸酯、倍他米松醋酸酯、泼尼卡酯、安西奈德、斯帕沙星、磺胺曲沙唑、磺胺甲嘧啶、妥布特罗、菲诺特罗、班布特罗、羟甲基克仑特罗等购自北京TRC公司。可的松、布地奈德、非那西丁、萘丁美酮、异丙安替比林、萘普生、氨基比林、甲芬那酸、酮洛芬、芬不芬、洛索洛芬、奥沙普秦、双氯芬酸钠、保泰松、吡罗昔康、美洛昔康、舒林酸、吲哚美辛、卡托普利、可乐定、氨苯蝶啶、普萘洛尔、阿替洛尔、美替洛尔、卡替洛尔、氯丙嗪、螺内酯、硝苯地平、尼群地平、吲达帕胺、依那普利、非洛地平、哌唑嗪、特拉唑嗪、尼索地平、卡维地洛、氨氯地平、尼莫地平、氯沙坦、贝那普利、缬沙坦、喹那普利、多沙唑嗪、尼卡地平、替米沙坦、恶喹酸、诺氟沙星、环丙沙星、培氟沙星、氧氟沙星、左氧氟沙星、莫西沙星、甲氧苄啶、磺胺甲恶唑、磺胺二甲嘧啶、磺胺嘧啶、磺胺间甲氧嘧啶、特布他林、沙丁胺醇、福莫特罗、沙美特罗等购自中国食品药品检定研究院。氟氢可的松醋酸酯、氢化可的松丁酸酯、曲安奈德醋酸酯、地夫可特、氟米松、氢化可的松戊酸酯、曲安西龙双醋酸酯、氟轻松醋酸酯等购自上海安谱公司。马布特罗购自德国WTEGA公司。磺胺多辛、磺胺间二甲氧嘧啶、磺胺二甲基异嘧啶购自美国Sigma公司。西马特罗购自北京振翔科技有限公司。巴洛沙星、加替沙星、洛美沙星、帕珠沙星、吡哌酸、氟罗沙星、磺胺吡啶购自中国药品生物制品检定所。乙腈、甲醇(色谱纯，德国Merck公司)；甲酸(色谱纯，天津科密欧公司)；实验用水为Milli-Q超纯水。
2方法与结果
2.1色谱条件
色谱柱：Agilent Pososhell 120EC-C18液相色谱柱(2.1mm×150mm，2.7μm)；柱温：40℃：流速：0.3mL/min；进样体积：10μL；流动相：A相为0.1％-甲酸水，B相为乙腈，梯度洗脱程序见表1。
表1流动相梯度洗脱程序
2.2质谱条件
电喷雾离子源(Electrospray ionization mass spectrometry conditions，ESI)；采集模式为预设定多反应监测模式(sMRM)；正离子模式下检测，离子源温度为550℃，喷雾电压：+5.5kV。目标化合物的详细质谱参数列于表2。
表2 132种目标分析物的sMRM参数
注：*为定量离子
2.3对照品溶液的配制
精密称取上述132种化学药物对照品适量，加甲醇溶解配制成质量浓度为1mg/mL的标准储备溶液，于-18℃冰箱中保存。分别适量精密量取各对照品储备液，加甲醇稀释成1μg/mL的混合标准工作液，于4℃冰箱内保存。
2.4供试品溶液的配制
将中成药或保健品药片1g研细混匀后，置于10mL容量瓶中，加入甲醇适量，超声10min，放冷，用甲醇定容至刻度，摇匀，过0.22μm滤膜，滤液待上机检测。
2.5标准曲线配制与线性范围
精密量取“2.3”项下配制的混合标准工作液适量，用甲醇配置成7个不同浓度(10μg/L、20μg/L、50μg/L、100μg/L、200μg/L、500μg/L、1000μg/L)混合标准溶液，现配现用。按“2.1”及“2.2”项下的色谱-质谱条件检测，以被测组分的峰面积为纵坐标，质量浓度为横坐标，进行线性回归，各化合物的回归方程、相关系数和线性范围见表3。
表3回归方程、相关系数、线性范围、检出限(LOD)和定量限(LOQ)
表中线性范围的单位是ng/mL，检出限的单位是ng/mL，定量限的单位是ng/mL。
2.6加标回收率及重复性实验
称取阴性样品18份于10mL容量瓶中，分别精密加入混合标准工作液适量，配制成50ng/mL、100ng/mL、1000ng/mL的低、中、高三个添加水平的加标样品，加入适量甲醇，静置20min后，按“2.4”项的操作描述对样品进行前处理，即得加标样品，每个添加水平制备6份平行样。按“2.1”和“2.2”项描述的色谱-质谱方法检测，采用外标法定量，通过标准曲线计算各化合物的含量，根据实际添加的化学药物量与测得化学药物量计算回收率。通过每个添加水平的6份平行样计算重复性。加标回收率及重复性结果见表4。
表4 132种化学药物回收率测定结果
3结论
3.1质谱条件的优化
在正离子模式下，使用针泵注射直接进样，通过质谱一级全扫描，确定各化学药物的母离子。在不同碰撞能下对各母离子进行子离子扫描，筛选出2个响应值高、稳定性好的子离子，随后对两对离子对进行MRM参数优化，得出针对每个子离子的最佳的去簇电压(DP)、碰撞电压(CE)和出口电压(CXP)。选出在最优条件下离子响应强的子离子作为定量离子，另一子离子作为定性离子。质谱采用的预设定多反应监测模式(sMRM)相比多反应监测模式(MRM)模式，可以实现同时检测更多的化合物并依然具有高灵敏度，极大的提高了检测通量，并有效的改善峰型，提高重现性。
3.2色谱条件的优化
分别考察了Agilent Poroshell 120EC-C18(100mm×2.1mm，2.7μm)、ThermoAcquity UPLC BEH C18(100mm×2.1mm，μm)色谱柱，结果显示EC-C18色谱柱具有更高的柱效，分离度更好，峰形更加尖锐对称，因此采用Agilent Poroshell 120EC-C18色谱柱进行分离。流动相分别测试了甲酸水(甲酸含量0.1％v/v)-甲醇体系、甲酸水(甲酸含量0.1％v/v)-乙腈体系及甲酸铵-甲酸水(甲酸含量0.1％v/v，甲酸铵含量5mmol/L)-乙腈。由于乙腈相比甲醇粘度低，所以在相同的梯度条件下使用乙腈作为有机相，目标化合物得到了更好的分离效果。当流动相中加入甲酸铵时，发现部分化合物会发生解离，造成色谱峰分裂，影响检测效果，所以最终确定甲酸水(甲酸含量0.1％v/v)作为水相。
3.3样品的提取
中成药和保健品片剂基质主要为淀粉、糖类、糊精和乳糖，相比动物源食品及化妆品基质更加干净，因此本发明在前处理方面不需除油脂等杂质，直接将药片研细，采用甲醇超声提取化学药物即可，同时选用甲醇作为提取溶剂，可避免提取到药片中的蔗糖，有效的保护色谱柱。
综上所述，本发明建立了高效液相色谱-串联质谱同时检测中成药和保健品中非法添加132种化学药物的快速检测方法。采用甲酸水(0.1％甲酸)-乙腈作为流动相，梯度洗脱模式，电喷雾正离子模式(ESI+)下检测。结果表明，132种化学药物线性关系良好，相关系数均大于0.995，三个添加水平的回收率在43.36％～114.92％之间，定量限在2μg/Kg～200μg/Kg之间。该方法灵敏度高，准确度好，检测通量大，耗时短，适合于中成药和保健品中非法添加化学药物的快速筛查，为打击非法添加及规范中成药和保健品市场，提供技术支持。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (8)
1.一种快速筛查中成药和保健品中非法添加的132种化学药物的方法，其特征在于，包括以下步骤：
一、溶液的配制
对照品溶液的制备：配制132种化学药物的混合标准溶液；
供试品溶液的配制：将待检测的中成药或保健品样品研细混匀，加入甲醇适量，超声处理，冷却，用甲醇定容，滤膜过滤，滤液待上机检测；
二、样品中132种化学药物的定性定量分析
1)将上述混合标准溶液用甲醇配置成个不同浓度混合标准溶液，进行高效液相色谱-串联质谱检测；以被测组分的峰面积为纵坐标，质量浓度为横坐标，进行线性回归，分别制作132种目标化学药物的标准曲线；建立132种化合物的回归方程、相关系数和线性范围；
所述高效液相色谱检测条件为：色谱柱为反相C18液相色谱柱；柱温：30～45℃；流速：0.2～0.4mL/min；进样体积：5～110μL；流动相：A相为0.05～0.2％v/v甲酸水，B相为乙腈，进行梯度洗脱；
所述串联质谱检测条件为：使用电喷雾离子源；采集模式为预设定多反应监测模式；在正离子模式下检测；132种化学药物的质谱参数分别为：
表中*为定量离子；
3)将上述配制好的供试样品溶液进行与混合标准溶液相同的高效液相色谱-串联质谱检测；根据标准曲线分别计算出样品中该132种目标化学药物的含量。
2.根据权利要求1所述的方法，其特征在于，所述对照品溶液中的溶剂为甲醇。
3.根据权利要求1所述的方法，其特征在于，所述供试品溶液的配制为：将待检测的中成药或保健品1g样品研细混匀，加入甲醇适量，超声处理5～15min，冷却，用甲醇定容至10～40mL，0.22μm滤膜过滤，滤液待上机检测。
4.根据权利要求1所述的方法，其特征在于，所述132种化合物的回归方程、相关系数和线性范围情况如下：
表中线性范围的单位是ng/mL，检出限的单位是ng/mL，定量限的单位是ng/mL。
5.根据权利要求1所述的方法，其特征在于，所述梯度洗脱的程序为：
其中，A相为0.08～0.12％v/v甲酸水，B相为乙腈。
6.根据权利要求1所述的方法，其特征在于，所述高效液相色谱检测条件为：色谱柱为Agilent Pososhell 120 EC-C18液相色谱柱；柱温：40℃；流速：0.3mL/min；进样体积：10μL；流动相：A相为0.1％v/v甲酸水，B相为乙腈。
7.根据权利要求1所述的方法，其特征在于，串联质谱检测时，离子源温度为500～600℃，喷雾电压：+5.0～+6.0kV。
8.根据权利要求1所述的方法，其特征在于，所述132种化学药物为非那西丁、萘丁美酮、异丙安替比林、萘普生、氨基比林、甲芬那酸、酮洛芬、芬布芬、洛索洛芬、奥沙普秦、双氯芬酸钠、保泰松、吡罗昔康、美洛昔康、舒林酸、吲哚美辛、泼尼松、可的松、氢化可的松、醋酸去氧皮质酮、甲基泼尼松龙、氟米龙、地塞米松、曲安西龙、醋酸泼尼松、醋酸泼尼松龙、醋酸可的松、氢化可的松醋酸酯、倍氯米松、氟米松、甲基泼尼松龙醋酸酯、氟米龙醋酸酯、氟氢可的松醋酸酯、布地奈德、氢化可的松丁酸酯、倍他米松醋酸酯、地塞米松醋酸酯、地夫可特、氢化可的松戊酸酯、倍他米松戊酸酯、曲安奈德醋酸酯、曲安西龙双醋酸酯、氯倍他松丁酸酯、泼尼卡酯、二氟拉松双醋酸酯、氟轻松醋酸酯、氟替卡松双丙酸酯、安西奈德、倍他米松双丙酸酯、康力龙、卡托普利、可乐定、氨苯蝶啶、普萘洛尔、阿替洛尔、美替洛尔、卡替洛尔、氯丙嗪、螺内酯、硝苯地平、尼群地平、吲达帕胺、依那普利、非洛地平、哌唑嗪、特拉唑嗪、尼索地平、卡维地洛、氨氯地平、尼莫地平、氯沙坦、贝那普利、缬沙坦、喹那普利、多沙唑嗪、尼卡地平、替米沙坦、萘啶酸、恶喹酸、西诺沙星、吡哌酸、帕珠沙星、诺氟沙星、依诺沙星、环丙沙星、培氟沙星、洛美沙星、丹诺沙星、氧氟沙星、马波沙星、左氧氟沙星、氟罗沙星、加替沙星、沙氟沙星、巴洛沙星、斯帕沙星、奥比沙星、双氟沙星、莫西沙星、磺胺吡啶、磺胺嘧啶、磺胺甲恶唑、磺胺噻唑、磺胺甲嘧啶、磺胺二甲基恶唑、磺胺二甲基异噁唑、磺胺曲沙唑、磺胺甲噻二唑、磺胺苯酰、磺胺二甲异嘧啶、磺胺二甲嘧啶、磺胺对甲氧嘧啶、磺胺间甲氧嘧啶、磺胺甲氧哒嗪、磺胺氯吡嗪、磺胺氯哒嗪、甲氧苄啶、磺胺喹恶啉、磺胺间二甲氧嘧啶、磺胺多辛、磺胺苯吡唑、磺胺硝苯、西马特罗、特布他林、妥布特罗、沙丁胺醇、羟甲基克仑特罗、菲诺特罗、马布特罗、福莫特罗、班布特罗、沙美特罗。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901780A (zh) * | 2012-10-17 | 2013-01-30 | 湖南省食品药品检验研究院 | 一种在中药、保健食品或化妆品中同时检测七种非法添加减肥类化学成分的方法 |
| CN103760245A (zh) * | 2013-12-18 | 2014-04-30 | 重庆市食品药品检验所 | 一种非法添加止咳平喘类化学成分的液-质多指标快速检测方法 |
| CN105158358A (zh) * | 2015-08-18 | 2015-12-16 | 江苏出入境检验检疫局动植物与食品检测中心 | 同时检测中成药和保健品中非法添加的42种化学药品的方法 |
-
2017
- 2017-11-20 CN CN201711154932.1A patent/CN108051534B/zh active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901780A (zh) * | 2012-10-17 | 2013-01-30 | 湖南省食品药品检验研究院 | 一种在中药、保健食品或化妆品中同时检测七种非法添加减肥类化学成分的方法 |
| CN103760245A (zh) * | 2013-12-18 | 2014-04-30 | 重庆市食品药品检验所 | 一种非法添加止咳平喘类化学成分的液-质多指标快速检测方法 |
| CN105158358A (zh) * | 2015-08-18 | 2015-12-16 | 江苏出入境检验检疫局动植物与食品检测中心 | 同时检测中成药和保健品中非法添加的42种化学药品的方法 |
Non-Patent Citations (2)
| Title |
|---|
| 刘芸 等: "高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法快速筛查中成药和保健食品中非法添加的42 种化学药物", 《分析化学》 * |
| 黄芳 等: "高效液相色谱-串联质谱法同时测定保健品及中成药中非法添加的17种壮阳类化学药", 《色谱》 * |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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