本文選題：嬰兒配方奶粉 + 飽和烴類礦物油(MOSH)　； 參考：《食品科學(xué)》2017年22期

【摘要】：建立嬰兒配方奶粉中飽和烴類礦物油(mineral oil saturated hydrocarbons,MOSH)的離線固相萃取(solid phase extraction,SPE)結(jié)合大體積進(jìn)樣-氣相色譜-氫火焰離子化檢測器(large volume injection-gas chromatographyflame ionization detection,LVI-GC-FID)的分析方法。該方法以正己烷為提取溶劑,提取液經(jīng)硝酸銀漬硅膠SPE柱凈化;通過比較不同長徑比SPE柱的凈化效果,確定以5 mL玻璃注射器作為分離MOSH的SPE柱,收集洗脫液5 mL,濃縮后注入LVI-GC-FID測定。GC的進(jìn)樣口升溫程序?yàn)?初始溫度45℃,保持1 min(分流比200∶1),以250℃/min升溫至360℃(分流閥關(guān)閉2 min),并保持27 min(分流比為100∶1);柱溫箱升溫程序?yàn)?35℃保持3 min,以25℃/min升溫至350℃,再以5℃/min升溫至370℃,保持10 min;FID溫度380℃;進(jìn)樣量40μL。結(jié)果表明:MOSH的標(biāo)準(zhǔn)品液體石蠟在2~500 mg/kg范圍內(nèi)呈良好線性關(guān)系,相關(guān)系數(shù)為0.999,方法的定量限為0.05 mg/kg,加標(biāo)回收率在92.62%~102.86%之間,相對標(biāo)準(zhǔn)偏差在0.85%~2.57%之間,適用于嬰兒配方奶粉中MOSH的定量分析。應(yīng)用該方法檢測市售10種嬰兒配方奶粉中的MOSH含量,其結(jié)果在0.24~1.30 mg/kg之間,其中MOSH(C16~C35)含量在0.12~0.85 mg/kg之間,表明有必要對嬰兒配方奶粉中的礦物油污染進(jìn)行監(jiān)管。
[Abstract]:An off-line solid phase extraction (solid phase extraction, SPE) of saturated hydrocarbon mineral oil (mineral oil saturated hydrocarbons, MOSH) in infant formula milk powder is established and the analytical method of mass injection gas chromatography hydrogen flame ionization detector (large volume injection-gas) is established. Methods with hexane as extraction solvent, the extraction solution was purified by SPE column with silver nitrate with silica gel. By comparing the purification effect of SPE column with different length and diameter ratio, 5 mL glass syringe was used as SPE column for separating MOSH, and 5 mL of eluent was collected. After concentrated injection LVI-GC-FID, the program of temperature rising of.GC at the initial temperature was 45, 1 min (distributary). Compared with 200: 1), heating up to 360 C at 250 /min (2 min), and maintaining 27 min (the shunt ratio of 100: 1), the temperature box of column temperature kept 3 min at 35 C, heating to 350 centigrade at /min at 35 degrees C, and then to 5 degrees /min to 370 degrees C, FID temperature, and L. results showed that MOSH's standard liquid paraffin wax was in 2~500 mg/kg There is a good linear relationship in the range, the correlation coefficient is 0.999, the method's quantitative limit is 0.05 mg/kg, the recovery rate is 92.62%~102.86%, the relative standard deviation is between 0.85%~2.57% and the quantitative analysis of MOSH in the infant formula milk powder. The method is used to detect the MOSH content in the 10 kinds of infant formula milk powder, and the result is in 0.24~1.3 The content of MOSH (C16~C35) is between 0.12~0.85 mg/kg and 0 mg/kg, indicating that it is necessary to supervise the pollution of mineral oil in infant formula.
【作者單位】： 北京市理化分析測試中心北京市食品安全測試工程技術(shù)研究中心北京市科學(xué)技術(shù)研究院分析測試技術(shù)重點(diǎn)實(shí)驗(yàn)室;國防科技大學(xué)西安通信學(xué)院;
【基金】：北京市科技計(jì)劃課題(Z161100000616005) 北京市科學(xué)技術(shù)研究院財(cái)政專項(xiàng)(PXM2016_178305_000013;PXM2017_178305_000001)
【分類號】：O657;TS252.51

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