›› 2013, Vol. 40 ›› Issue (S1): 71-74.

• 安全检测 • 上一篇    下一篇

利用对β-谷甾醇含量的检测鉴别生鲜乳中掺假植物脂肪的研究

魏雪冬, 姜毓君, 石馨, 刘波, 于力涛, 王象欣, 单艺   

  1. 东北农业大学, 国家乳制品质量监督检验中心, 黑龙江哈尔滨 150028
  • 收稿日期:2013-08-01 出版日期:2013-09-30 发布日期:2013-11-29
  • 通讯作者: 王象欣
  • 作者简介:魏雪冬(1973-),男,黑龙江人,硕士,工程师,研究方向:食品质量检测。

The Research on the Plant Fat Adulteration in Raw Milk by Determination of β-sitosterol

WEI Xue-dong, JIANG Yu-jun, SHI Xin, LIU Bo, YU Li-tao, WANG Xiang-xin, SHAN Yi   

  1. The National Dairy Testing Center, Northeast Agricultural University, Harbin 150028, China
  • Received:2013-08-01 Online:2013-09-30 Published:2013-11-29

摘要: 本试验建立了气相色谱―质谱法测定生鲜乳中β-谷甾醇的检测方法,由于理论研究表明生鲜乳中的乳脂肪是动物油脂,不应含有或很少含有植物油脂中特有的甾醇β-谷甾醇,因此对多个地区生鲜乳中β-谷甾醇的本底含量进行分析,给出生鲜乳中掺假植物油脂的鉴定方法。用质量比1.25的氢氧化钾水溶液25 mL皂化样品,100 mL维生素C的乙醇溶液作为稳定剂和抗氧化剂,皂化液用石油醚和乙醚萃取,转溶剂至甲苯,离心进样质谱。选用高柱效的60 m DB-5毛细管柱,进样量1 μL,程序升温在35 min内实现β-谷甾醇与其他醇类及杂质的良好分离。选择离子414定量,检出限为0.10 mg/L,线性相关系数r=0.9991。运用该方法对6个地区生鲜乳中β-谷甾醇含量进行检测,结果得到最高值为0.86 mg/L,常见植物油中β-谷甾醇的含量为1~3 g/L。表明生鲜乳中利用植物脂肪代替乳脂肪时,每提高1%植物脂肪将多产生最少相当于本底量12倍的β-谷甾醇,从而判定生鲜乳中是否掺假植物脂肪。

关键词: 乳脂肪掺假; β-谷甾醇; 气相色谱―质谱法

Abstract: A gas chromatography-mass spectrometric (GC-MS) method was established for the determination of β-sitosterol in raw milk. Theoretical studies had shown that the fat in raw milk belonged to animal fat, fresh milk should not contain plant oils or rarely contain phytosterols,especially β-sitosterol. Based on the analysis of the content of β-sitosterol in raw milk from different area,the identical method of mixing plant oil in raw milk had been given. Using the mass ratio of KOH aqueous solution of 1.25 of the 25 mL saponificate sample,100 mL vitamin C ethanol solution as stabilizer, liquid saponification with petroleum ether and diethyl ether,turn solvent to toluene,centrifugal inlet mass spectrometry. Selecting 60 m DB-5 capillary column with high column efficiency,the injection volume was 1 μL,programmed raising temperature to achieve a good separation of β-sitosterol and other alcohols and impurities within 35 minutes. Selected ion 414 quantitative,the detection limit was 0.10 mg/L. The linear correlation coefficient r was 0.9991. Using this method to detect β-sitosterol content in fresh milk from 6 different regions,the highest content was 0.86 mg/L,the content of β-sitosterol common plant oil were 1 to 3 g/L. In conclusion,using plant fat replace dairy fat,and each one percent of plant fat would produce β-sitosterol as 12 times as the milk without plant fat at least. Thus,mixing plant fat could be identified in raw milk.

Key words: dairy fat adulteration; β-sitosterol; GC-MS

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