Method for determining polyamines in urine
A determination method and urine technology, applied in the field of medicine, can solve the problems of low body content and incomplete establishment of a polyamine detection method, and achieve the effects of good repeatability, reduction of side reactions, and easy operation.
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Embodiment 1
[0036] (1) Urine sample pretreatment
[0037] a. Take 500 μL of urine sample and add 5% HClO 4 250 μL, vortex to mix, and centrifuge.
[0038] b. Take the supernatant after treatment in step a, add 2 mol mL -1 NaOH 800 μL, 250 μL benzoyl chloride mass concentration of 4% mixed solution of benzoyl chloride and acetonitrile, vortex to dissolve and mix well, 30 o C. Ultrasonic reaction for 30 min, adding 1 mL of saturated sodium chloride solution to terminate the reaction, extracting the derivatized polyamine with 4 mL of ether, drying under air flow, reconstitution with 100 μL of methanol, centrifuging at 15000 r.m.p for 3 min, and taking 20 μL The supernatant was analyzed by LC-MS.
[0039] (2) Liquid phase separation: the chromatographic column is Kromasil C 18 Column (250 mm×4.6 mm, 5 μm); mobile phase A: methanol, B: water; gradient elution: 0-14 min: 55 % A→74 % A. Flow rate is 1.0 mL ? min -1 , the column temperature is 35 o c.
[0040] (3) MS measurement
[0...
Embodiment 2
[0046] (1) Urine sample pretreatment
[0047] a. Take 500 μL of urine sample and add 9% HClO 4 250 μL, vortex, and centrifuge.
[0048] b. Take the supernatant after treatment in step a, add 0.5 mol mL -1 NaOH 800 μL, 250 μL benzoyl chloride mass concentration of 4% mixed solution of benzoyl chloride and acetonitrile, vortex to dissolve and mix well, 30 o C. Ultrasonic reaction for 30 min, adding 1 mL of saturated sodium chloride solution to terminate the reaction, extracting the derivatized polyamine with 4 mL of ether, drying under air flow, reconstitution with 100 μL of methanol, centrifuging at 15000 r.m.p for 3 min, and taking 20 μL The supernatant was analyzed by LC-MS.
[0049] (2) Liquid phase separation: the chromatographic column is Kromasil C 18 Column (250 mm×4.6 mm, 5 μm); mobile phase A: methanol, B: water; gradient elution: 0-14 min: 55 % A→74 % A. Flow rate is 1.0 mL ? min -1 , the column temperature is 35 o C, inject 20 μL.
[0050] (3) MS measurem...
Embodiment 3
[0056] (1) Urine sample pretreatment
[0057] a. Take 500 μL of urine sample and add 5% HClO 4 250 μL, vortex to mix, and centrifuge.
[0058] b. Take the supernatant after treatment in step a, add 2 mol mL -1 NaOH 800 μL, 250 μL benzoyl chloride mass concentration of 1% mixed solution of benzoyl chloride and acetonitrile, vortex to dissolve and mix well, 30 o C. Ultrasonic reaction for 30 min, adding 1 mL of saturated sodium chloride solution to terminate the reaction, extracting the derivatized polyamine with 4 mL of ether, drying under air flow, reconstitution with 100 μL of methanol, centrifuging at 15000 r.m.p for 3 min, and taking 20 μL The supernatant was analyzed by LC-MS.
[0059] (2) Liquid phase separation: the chromatographic column is Kromasil C 18 Column (250 mm×4.6 mm, 5 μm); mobile phase A: methanol, B: water; gradient elution: 0-14 min: 55 % A→74 % A. Flow rate is 1.0 mL ? min -1 , the column temperature is 35 o C, inject 20 μL.
[0060] (3) MS mea...
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