| ObjectivesFood safety is closely related to human health.Foodborne diseases caused by food contamination are one of the most common health problems in the world today.patulin is a mycotoxin that causes foodborne diseases.In this study,a HPLC method was established for the determination of patulin in fruits and their products,and the situation of patulin in apple,hawthorn and their products was investigated and analyzed,so as to understand the situation of patulin in apple,hawthorn and their products,and to explore the factors affecting food safety related to consumers.Method1.To establish a method for the detection of patulin in fruits and their productsThe homogenized samples were enzymolized with pectinase(no pectinase was used for the liquid samples),extracted with ethyl acetate,concentrated to dry in a water bath at 40℃with a rotary evaporator,dissolved with acetic acid solution,mixed with acetonitrile for purification,purified liquid nitrogen blown to near dry,redissolved,and detected by high performance liquid chromatography.The HPLC conditions for the determination of patulin were explored by selecting suitable column type and composition and proportion of mobile phase.The established method was verified from four aspects:linearity,accuracy,precision and detection limit.2.Investigation and analysis of patulin in fruit and its products2.1 Sample collection methodFrom September 2021 to January 2022,various online shopping platforms and supermarkets,convenience stores and farmers’ markets in Jinan,Shandong Province were selected as sampling points to conduct random sampling of apple,hawthorn and their products.2.2 Type and quantity of samplesA total of 410 samples were tested,including 50 apples,50 apple juice,50 apple puree,50 applesauce,50 hawthorn,50 hawthorn juice,50 hawthorn slices,50 hawthorn roll,and 10 other hawthorn products(hawthorn soup,dried hawthorn,etc.).3.Analysis of influencing factors of food safetyThe influencing factors of food safety were analyzed from the perspective of consumers’food purchase,and the influencing factors of food safety were finally determined to include sample types(Sample type 1:apple juice,hawthorn juice,apple puree,applesauce,hawthorn slices,hawthorn roll,apple,hawthorn,other hawthorn products;sample type 2:apple and its products,hawthorn and its products;sample type 3:fruit,fruit products;sample type 4:fruit juice,canned fruit,preserves,fruit),sampling site,origin,and then correlation analysis was conducted between each influencing factor and the detected situation and detected content of patulin.4.Data analysisExcel and SPSS24.0 software were used for data analysis to calculate the corresponding detection rate or over standard rate,and chi-square test,bivariate Spearman correlation analysis,non-parametric test of two independent samples,and non-parametric test of multiple independent samples were respectively carried out for the detection situation and detection concentration of patulin and the influencing factors.To explore whether the influencing factors are related to patulin in food,in order to P<0.05 was considered statistically significant.Results1.Establishment and verification of high performance liquid chromatography for determination of patulin in fruit and its products1.1 Chromatographic conditionsThe column was C18(250×4.6mm,5μ).Mobile phase:acetonitrile(A)-0.8%tetrahydrofuran(B),gradient elution condition:0min～11min,95%B;12min,0%B;13min～26.5min,95%B;Detection wavelength:276 nm;Column temperature 40℃;Flow rate:0.8mL/min.1.2 Linear RelationshipThe regression equation is Y=508.24X-12.229 and R2 is 0.9999.1.3 AccuracyThe recoveries of patulin were 80.06%-97.51%in three kinds of solid and semi-fluid samples with different spiked concentrations,and 91.70%-96.72%in three kinds of liquid samples with different spiked concentrations.1.4 PrecisionThe peak area values of precision test were 9782,9811,9671,9869,9639,respectively.9705,RSD was 0.91%.1.5 Detection LimitUnder the experimental conditions,the detection limit of solid and semi-fluid samples was 0.32μg/kg,the limit of quantitation was 1.05μg/kg,the detection limit of liquid samples was 0.17μg/kg,the limit of quantitation was 0.55μg/kg.2.Investigation and analysis of patulin in fruit and its products2.1 Detection rate and detection range of patulinIn 410 samples,the detection rate of PAT was 80%,the detection range was 0.64～125.95μg/kg,and the over standard rate was 0.49%.The PAT detection rate from high to low was apple(98%)and hawthorn slices(98%),hawthorn(94%),apple puree(90%)and other hawthorn products(90%),hawthorn juice(84%),hawthorn roll(74%),applesauce(68%),apple juice(32%).2.2 Test results of Apple samplesThe detection rate of PAT in apple and its products was 72%,and the content of PAT in apple and its products was 0.66～37.60μg/kg.2.3 Test results of hawthorn samplesThe detection rate of PAT in hawthorn and its products was 87.62%,the over standard rate was 0.95%,and the detected content ranged from 0.64 to 125.95μg/kg.2.4 Test results of different placesThe detection rate of PAT in domestic samples was 82.6%,the over standard rate was 0.56%,and the detected content ranged from 0.64 to 125.95μg/kg.The detection rate of imported samples was 57.6%,and the content range was 1.37～11.18μg/kg.2.5 Detection results of different sampling pointsThe PAT detection rate from high to low was offline convenience stores(100%),farmers’markets(90%),offline supermarkets(80.75%),and online shopping platforms(76.38%).The detection range of penicillin in the samples collected from offline convenience stores was 0.73～7.18μg/kg.The range of detected content in the farmers’ market was μg/kg.The detected content in offline supermarkets ranged from 1.26 to 18.5μg/kg.The detection range of online shopping platform is 0.64～125.95μg/kg.3.Analysis of food safety influencing factors3.1 Correlation analysis between influencing factors and detected situationThe influencing factors of food safety were analyzed from the perspective of consumers’food purchase,and the influencing factors of food safety were finally determined to include sample types(Sample type 1:apple juice,hawthorn juice,apple puree,applesauce,hawthorn slices,hawthorn roll,apple,hawthorn,other hawthorn products;sample type 2:apple and its products,hawthorn and its products;sample type 3:fruit,fruit products;sample type 4:fruit juice,canned fruit,preserves,fruit),sampling site,origin.Among the influencing factors,sample type 1,sample Type 2,sample Type 3,sample type 4 and the place of origin were significantly correlated with the detected situation,and there was a significant correlation with the detected content.Sample type 3 and the place of origin were positively correlated with the detected situation,sample type 1,sample type 2 and sample type 4 were negatively correlated with the detected situation.3.2 Non parametric test of influencing factors and detected contentsThe distribution of detected content was different for sample type 1 and sample type 4(fruit juice,canned,preserved fruit,fruit).For sample type 2 and sample type 3,the range of detected content is different,and the distribution of detected content is different in the origin and the category of sampling point.ConclusionA high performance liquid chromatography method with high sensitivity,good repeatability and high accuracy was established for the determination of patulin in fruit and its products.The detection rate of patulin displayed in apple and hawthorn slices was high,while the detection rate of patulin displayed in apple juice was low,the excess rate of patulin displayed in fruits and products sold on online shopping platforms and in Jinan City was low,and the food safety situation was good.Relevant food safety departments can strengthen the supervision and management of food safety from sample type,origin and other influencing factors. |
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