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超高效液相色谱-三重四级杆质谱法用于阿胶糕类食品中阿胶的鉴别及马、牛、羊、猪皮源成分的检测

2019-09-10张静娴胡青董洪霜孙健冯睿于泓张甦毛秀红季申

世界中医药 2019年4期
关键词:特征检测

张静娴 胡青 董洪霜 孙健 冯睿 于泓 张甦 毛秀红 季申

摘要 目的:建立以特征肽为检测指标的阿胶糕中阿胶的鉴别方法与马皮、牛皮、羊皮、猪皮源成分的检测方法。方法:采用三氯乙酸沉淀法提取阿胶糕中的蛋白质,胰蛋白酶进行酶解处理,利用超高效液相色谱-三重四级杆质谱法(UHPLC-QQQ MS),电喷雾离子源(ESI),正离子模式下扫描,采用多重反应监测模式,对特征肽目标离子进行检测。结果:经验证,鉴别方法和检查方法均均有良好的专属性,灵敏度高。市售样品测定结果显示,部分样品中检出阿胶成分,有的样品中检出牛皮源成分,有的样品中未检出任何皮源性成分。结论:所建立方法操作简便,专属性强,可用于阿胶糕中阿胶的鉴别和掺假杂皮胶的检测。

关键词 阿胶;阿胶糕;超高效液相色谱-三重四级杆质谱法;多重反应检测;特征肽;蛋白质组学技术;胶原蛋白

Development of UHPLC-QQQ MS Method for Identification of Donkey-hide Gelatin Cake and Detection of Constituents from Horse,Ox,Sheep or Pig Skin

Zhang Jingxian,Hu Qing,Dong Hongshuang,Sun Jian,Feng Rui,Yu Hong,Zhang Su,Mao Xiuhong,Ji Shen

(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

Abstract Objective:To establish a method for the identification of colla corii asini in donkey-hide gelatin cake and the detection of constituents from horse,ox,sheep or pig skin with characteristic peptide as the detection marker.Methods:The protein was extracted by trichloroacetic acid precipitation method,and trypsin was used for enzymatic hydrolysis.UHPLC-QQQ MS was used with electrospray positive ionization mode and multiple reaction monitoring(MRM)to detect the target ions.Results:The method was validated to be specific and sensitive.The results showed that some samples were found to be containing colla corii asini and some samples containing bovine skin ingredients,whereas some samples did not detect any skin-derived constituents.Conclusion:The established method was validated to be simple and specific.It can be used for identification of colla corii asini in donkey-hide gelatin cake and detection of adulteration.

Key Words Colla corii asini; Donkey-hide gelatin cake; UHPLC-QQQ MS; MRM; Characteristic peptide; Proteomics; Collagen

中圖分类号:R284.1文献标识码:Adoi:10.3969/j.issn.1673-7202.2019.04.008

阿胶糕是以阿胶、黑芝麻、核桃仁等为主要原料,添加冰糖、黄酒等辅料,经配料、熬制等过程制成的可以即食的产品。阿胶具有补血养气、美容养颜、润肠通便、抗衰老、提高免疫力的综合保健功效,可用于失血贫血、缺铁贫血、再生障碍性贫血等[1-6]。

近年来,随着人民生活水平的提高和保健意识的增强,阿胶市场逐年扩大,阿胶糕具有食用方便,口感好的特点,迅速在市场上崛起。随着阿胶市场的扩大,阿胶原料驴皮资源短缺,价格上涨,部分生产企业为降低成本,采用马、骡、牛、羊等价格相对低廉的皮制造阿胶,生产阿胶糕类食品,严重影响着患者和消费者的饮食用药安全。……

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