摘要
餐具清洗时洗涤剂易产生氯酸盐残留,对人体健康造成危害。试验建立一种超高效液相色谱-串联质谱法(UPLC-MS/MS)测定餐具洗涤剂及清洗后餐具表面氯酸盐含量。以0.2%甲酸水溶液为提取液,用正己烷去除洗涤剂中表面活性剂,餐具表面的氯酸盐用WAX柱富集,采用乙腈和20 mmol/L甲酸铵溶液作为流动相梯度洗脱,超高效液相色谱-串联质谱仪测定,内标法定量。结果表明,氯酸盐在0.2~500 ng/mL范围内线性关系良好(r=0.999 7)。该方法中,餐具洗涤剂的氯酸盐检出限为2.0μg/kg,定量限为6.0μg/kg,在阴性样品中分别以1, 2和10倍定量限做加标试验,平均回收率分别为91.27%, 97.94%和101.07%,平均相对标准偏差分别为2.02%, 6.06%和6.14%(n=6)。餐具清洗后表面氯酸盐残留的检出限为0.05μg/L,定量限为0.15μg/L,在阴性样品中分别以1, 2和10倍定量限做加标试验,平均回收率分别为88.00%, 97.47%和103.67%,平均相对标准偏差分别为1.82%, 2.60%和4.26%(n=6)。该方法灵敏度和精密度较高,线性关系良好,检测效率较高,具有较好的应用前景。
Chloride residues on tableware caused by the use of detergent has became a potential risk to human health.An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method is established to determine the content of chloroate in tableware detergent and tableware surface.Targeted samples are first extracted with 0.2%methanoic acid solution using an ultrasound followed by purification through a WAX solid phase extraction column,removing surfactants with Normal hexane.Acetonitrile and 20 mmol/L methyl ammonium solution are selected as the mobile phase for the course of gradient elution in UPLC-MS/MS,and the target samples are quantified by the internal standard method.The obtained chart for chloride gives a good linear relationship in the concentration range of 0.2-500 ng/mL(r-0.9997).In this method,the limit of detection of chlorate in detergent is 2.0μg/kg,and the limit of quantitation is 6.0μg/kg.The negative samples are tested at 1,2 and 10 times of the limit of quantification,and the recoveries are 91.27%,97.94%and 101.07%,with the relative standard deviations of 2.02%,6.06%and 6.14%,respectively(n=6).The limit of detection of chloroate residues in the tableware surface after detergent administration is 0.05μg/L,and the limit of quantitation is 0.15μg/L.The negative samples are tested at 1,2 and 10 times of the limit of quantification,and the recoveries are 88.00%,97.47%and 103.67%,with the relative standard deviations of 1.82%,2.60%and 4.26%,respectively(n-6).The advantages of simple pretreatment,high accuracy,sensitivity and stability are shown in this method,indicating good application prospects.
作者
梁钰莹
唐楚林
汤曜名
李锦清
LIANG Yuying;TANG Chulin;TANG Yaoming;LI Jinqing(Guangdong Testing Institute of Product Quality Supervision,Foshan 528300)
出处
《食品工业》
CAS
2023年第9期297-301,共5页
The Food Industry
