化学分析计量
化學分析計量
화학분석계량
CHEMICAL ANALYSIS AND METERAGE
2015年
1期
68-70
,共3页
液相色谱串联质谱法%复硝酚钠%残留%水果
液相色譜串聯質譜法%複硝酚鈉%殘留%水果
액상색보천련질보법%복초분납%잔류%수과
UPLC-MS/MS%compound sodium nitrophenolate%residue%fruit
以甲醇提取样品,采用超高效液相色谱串联质谱法(UPLC–MS/MS)测定水果中复硝酚钠的残留量。以甲醇–10 mmol/L乙酸铵水溶液(体积比为60∶40)为流动相,质谱采用电喷雾负离子MRM检测模式。对硝基苯酚钠和5-硝基愈创木酚钠的线性范围为0.05~2.00 mg/L,检出限为0.01 mg/kg,邻硝基苯酚钠的线性范围为2.5~100.0 mg/L,检出限为0.5 mg/kg,线性相关系数均大于0.995。实际样品中对硝基苯酚钠、邻硝基苯酚钠和5-硝基愈创木酚钠的加标回收率分别为83.0%~93.4%,81.0%~87.4%,83.0%~91.8%,测定结果的相对标准偏差小于7%(n=6)。该法操作简单、快捷,精密度、准确度高,适用于水果中复硝酚钠的残留分析。
以甲醇提取樣品,採用超高效液相色譜串聯質譜法(UPLC–MS/MS)測定水果中複硝酚鈉的殘留量。以甲醇–10 mmol/L乙痠銨水溶液(體積比為60∶40)為流動相,質譜採用電噴霧負離子MRM檢測模式。對硝基苯酚鈉和5-硝基愈創木酚鈉的線性範圍為0.05~2.00 mg/L,檢齣限為0.01 mg/kg,鄰硝基苯酚鈉的線性範圍為2.5~100.0 mg/L,檢齣限為0.5 mg/kg,線性相關繫數均大于0.995。實際樣品中對硝基苯酚鈉、鄰硝基苯酚鈉和5-硝基愈創木酚鈉的加標迴收率分彆為83.0%~93.4%,81.0%~87.4%,83.0%~91.8%,測定結果的相對標準偏差小于7%(n=6)。該法操作簡單、快捷,精密度、準確度高,適用于水果中複硝酚鈉的殘留分析。
이갑순제취양품,채용초고효액상색보천련질보법(UPLC–MS/MS)측정수과중복초분납적잔류량。이갑순–10 mmol/L을산안수용액(체적비위60∶40)위류동상,질보채용전분무부리자MRM검측모식。대초기분분납화5-초기유창목분납적선성범위위0.05~2.00 mg/L,검출한위0.01 mg/kg,린초기분분납적선성범위위2.5~100.0 mg/L,검출한위0.5 mg/kg,선성상관계수균대우0.995。실제양품중대초기분분납、린초기분분납화5-초기유창목분납적가표회수솔분별위83.0%~93.4%,81.0%~87.4%,83.0%~91.8%,측정결과적상대표준편차소우7%(n=6)。해법조작간단、쾌첩,정밀도、준학도고,괄용우수과중복초분납적잔류분석。
Samples were extracted by methanol,the compound sodium nitrophenolate residues in fruit were detected by ultra performance liquid chromatography tandem mass spectrometry (UPLC/MS/MS). With mobile phase of methanol–10 mmol/L ammonium acetate solution (volume ratio was 60∶40),the mass spectrometry was operated in the positive ion mode of multiple reaction monitoring. The linear range of o-nitrophenol sodium and 5-nitroguaiacol sodium was 0.05–2.00 mg/L, the detection limit was 0.01 mg/kg. The linear range of p-nitrophenol sodium was 2.5–100.0 mg/L, and the detection limit was 0.5 mg/kg, the linear correlation coefficients were more than 0.995. The average recoveries of p-nitrophenol sodium, o-nitrophenol sodium and 5-nitroguaiacol sodium were 83.0%–93.4%,81.0%–87.4%, 83.0%–91.8%,respectively,and the relative standard deviation of detectiong results was less than 7%(n=6). The method is simple,rapid, precise, and accurate, which is suitable for determination of compound sodium nitrophenolate in fruits.