| Function food is belong to the field of food, it has a special of food, and with a specific health function. Known as dietary supplement in the United States, called improve food in Germany, referred to function food in Japan, and referred health food in China. According to the role by regulating body functions can be divided into:regulating immune function, anti-aging, fatigue, weight loss, improve memory, regulate blood sugar and so on. Its basic principle isn’t produce any acute, subacute or chronic damage to the human body. But some enterprises illegally added chemicals ingredients in such foods in order to pursue their own interests. After taking these functional food, not only can’t play a role in health care for the body, but also it will harm to health.At present, the phenomenon of illegal added pharmaceutical ingredients in function foods, including the following:first, add anti-inflammatory drugs in the anti-rheumatic health food; second, add exeited drugs in the reducing weight health food; third, add hypoglycemic drugs in the glucose regulation health food; four, add hormone drugs in the anti-fatigue health food; five, add antipsychotic drugs or β-blockers drugs in the sedative health food. Front three cases have been related research, this article centers on study behind two cases.This study based on the sample pretreatment method, quantitative method and instrument analysis conditions were systematically optimized, established UPLC-MS/MS analysis method for the determination of 30 hormones in anti-aging functional foods and 11 P-blockers in sedative functional foods, respectively. The method has a good sensitivity, accuracy, stability and reliability.The full text is made up of two parts.Part I Simultaneous determination of 30 hormones in anti-aging function food by UPLC-MS/MSObjective:A novel analytical method was developed for the simultaneous determination of 30 hormones in anti-aging functional foods using UPLC-MS/MS. Methods:The analytes were extracted with acetic acid-acetonitrile (1:99,v/v), methanol and acetone by ultrasound, respectively. The extract was concentrated to dryness, dissolved in formic acid-methanol-methylene chloride (0.1:20:80,v/v/v), cleaned-up and concentrated on an ENVI-Carb/NH2 SPE column. After the eluent to dryness under nitrogen gas stream,1mL methanol-water(1:1,v/v) to dissolve the residue. The analytes were separated on an Shim-pack XR-ODS Ⅱ (2.0×150mm,2.0μm), positive ion electrospray mode was eluted by gradient with acetonitrile and 2 mmol/L ammonium acetic (include 0.2% formic acid); negative ion electrospray mode was eluted by gradient with acetonitrile and water. The flow rate was 0.3 mL/min, the column temperature was 40℃ and the injection volume was 30 μL. Mass spectrometry conditions of positive ion electrospray mode:electrospray voltage 5.5 kV; atomization gas pressure 0.38 MPa; air curtain gas pressure 0.33 MPa; assist gas pressure 0.34 MPa; ion source temperature 650℃; Collision room entrance voltage 10 V. Mass spectrometry conditions of positive ion electrospray mode:electrospray voltage -4.5kV; atomization gas pressure 0.21MPa; air curtain gas pressure 0.16 MPa; assist gas pressure 0.24 MPa; ion source temperature 550℃; Collision room entrance voltage -10V. Quantified by a matrix-matched standard curve. Results: There were good linear relationships in the range of 1.0-1000.0 μg·L-1(r2≥0.9900).The limit of detection of 30 hormones were 0.02～1.43μg·kg-1, limits of quantification were 0.09～4.76μg·kg-1.The recoveries were between 72.2%～123.6% for the high, middle and low concentration, and the RSD were less than 15.0%. Conclusion:This method has high accuracy and high sensitivity, which can be used to determine hormone illegal adding to anti-aging function food.Part II Simultaneous determination of 11 β-blockers in sedative function food by UPLC-MS/MSObjective:Establishment a UPLC-MS/MS method for the determination and confirmation of 11 β-blockers in sedative function food. Methods:The samples were extracted twice with acetic acid-acetonitrile-methanol (0.1:3:7,v/v/v) by shake, the extracts was purified with the mixed QuEchERS adsorbents, and to dryness under nitrogen gas stream, reconstitution with acetonitrile-water(3:7,v/v) before the analysis by UPLC-MS/MS.The analytes were separated on a Acquity UPLCTM BEH C18 (100 mm×2.1 mm,1.7μm), positive ion electrospray mode was eluted by gradient with acetonitrile and 2 mmol/L ammonium acetic (include 0.2% formic acid). And the flow rate was 0.3 mL/min, the column temperature was 40℃ and the injection volume was 5μL. Conditions of MS/MS:electrospray voltage 5.5 kV; atomization gas pressure 0.45 MPa; air curtain gas pressure 0.21 MPa; assist gas pressure 0.41 MPa; ion source temperature 650℃; Collision room entrance voltage 10V. Tandem mass spectrometric detection was performed with a positive electrospray ionization (ESI+) source. The method used isotope internal standard quantitation. Results:Good linear relationship (r≥0.9990) was observed within the concentration range of 1.0～500.0μg·L-1. The limit of detection of 11 P-blockers were 0.02～0.16μg·kg-1, limits of quantification were 0.07～0.54μg·kg-1.At spiking levels of 3.0,7.5 and 15.0 μg·kg-1 in different matrices, average recoveries were between 71.8%～121.9%,with the RSD were less than12.6%. Conclusion:The method is novel, reliable, sensitive with wide linearity range, and strong practicability, which can be used for qualitative and quantitative analysis of β-blockers in sedative function food. |
PDF Full Text Request