【摘要】：建立了銀漬硅膠固相萃取柱離線(Ag-SPE)凈化,程序升溫進(jìn)樣-氣相色譜-氫火焰離子化檢測(cè)器(PTV-GC-FID)定量分析巧克力中飽和烷烴礦物油(MOSH)的方法。以正己烷浸泡提取巧克力中的MOSH,離心后取1 mL上清液,過(guò)0.3%Ag漬硅膠SPE柱凈化,氮吹濃縮,定容至0.2 mL,注入GC分析;GC的進(jìn)樣口程序升溫過(guò)程: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100∶1);進(jìn)樣量40μL;柱溫箱升溫程序?yàn)?35℃保持3 min,以25℃/min升溫至350℃,以5℃/min升溫至370℃,保持10 min,載氣為高純氮?dú)?流速1.3 mL/min(壓力60 k Pa);FID溫度為380℃。結(jié)果表明,本方法的MOSH定量限為0.5 mg/kg,加標(biāo)回收率為84.9%~108.6%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為0.2%~1.5%。運(yùn)用本方法對(duì)25個(gè)市售巧克力樣品中的MOSH含量進(jìn)行了測(cè)定,3個(gè)樣品未檢出,其余22個(gè)樣品中MOSH含量為1.09~8.15 mg/kg(其中C_(16)~C_(35)的含量為0.56~4.43 mg/kg),有3個(gè)樣品含量高于5.00 mg/kg,為嚴(yán)重污染樣品。本方法操作簡(jiǎn)便,檢出限低,適用于巧克力中MOSH的定量測(cè)定。
[Abstract]:A method for the determination of (MOSH) in saturated alkane mineral oil in chocolate by temperature-programmed injection gas chromatography-hydrogen flame ionization detector (PTV-GC-FID) has been established by using silver silica gel solid phase extraction column off-line (Ag-SPE) purifying and temperature-programmed injection-gas chromatography-hydrogen flame ionization detector (PTV-GC-FID). One mL supernatant was extracted by centrifugation with MOSH, extracted from chocolate with n-hexane immersion. The supernatant was purified by 0.3%Ag silica gel SPE column, then concentrated by nitrogen blow, and then injected into GC at a constant volume of 0.2 mL,. The process of GC injection programmed temperature is as follows: initial temperature 45 鈩，

本文編號(hào)：2345465