Solid phase extraction method for detection of aldicarb and its metabolites in ginger
Solid phase extraction method for the detection of aldicarb and its metabolites in ginger (SilibaseTM NH2 )
First, the purpose of the experiment
In this study, solid phase extraction was used as a pretreatment method for ginger samples, and LC-MS/MS method was used as a detection method. The method can simplify the pretreatment process of the sample, save the use of organic solvents, and is easy to operate.
Second, the experimental target
Three aldicarb and its metabolite standards: aldicarb (CSA: 116-06-03), aldicarb sulfone (CSA: 1646-88-4), aldicarb sulfoxide (CSA: 1646-87) -3).
Third, the scope of application
The method is applicable to the detection and confirmation of aldicarb, aldicarb sulfone and aldicarb sulfoxide LC-MS/MS in samples of ginger, rice and peanut.
Fourth, the reference standard
Import and export industry standard "SN/T 2441-2010 Determination of aldicarb, aldicarb sulfone and aldicarb sulfoxide residues in imported and exported foods by liquid chromatography-mass spectrometry/mass spectrometry.
V. Experimental materials
SilibaseTM NH2 solid phase extraction column 3mL/500mg.
Sixth, experimental methods
1, sample extraction
Weigh 5.0g sample (accurate to 0.01g) in a 50mL centrifuge tube, add 20mL acetonitrile, homogenize for 2min, shake and extract for 20min, the supernatant is collected into the separatory funnel through anhydrous sodium sulfate, and the residue is added with 20mL acetonitrile. The above operation was repeated once, the filtrate was combined twice, 20 mL of n-hexane saturated with acetonitrile was added, the mixture was shaken for 10 min, the layer was allowed to stand, the n-hexane layer was discarded, and the acetonitrile layer was concentrated by rotary evaporation to dryness at 40 ° C, using 2 mL of methanol - Dichloromethane (1:99, by volume) was dissolved and to be purified.
2, SPE column purification
(1) Activation: Activation was carried out by adding 5 mL of methanol-dichloromethane (1:99, by volume), and the effluent was discarded.
(2) Loading: Add the liquid to be purified, the flow rate is controlled within 1 mL/min, and the effluent is collected.
(3) Elution: Elution was carried out with 5 mL of methanol-dichloromethane (1:99, by volume), and the effluent was received and repeated once, and the effluent of steps (2) and (3) was combined.
(4) Concentration and constant volume: 40 ° C under a slow nitrogen flow to near dry (about 0.5 mL), then evaporated, with 1.0 mL of acetonitrile -0.1% aqueous formic acid (10:90, volume ratio) to a volume of 1 mL, Pass through a 0.45 μm micropore filter on LC-MS/MS to be determined.
3. LC-MS/MS conditions
Column: Venusil ASB C18 (2.1 × 150mm, 5μm, 100Å)
Mass spectrometer: API 4000
A: acetonitrile solution; B: 0.05% formic acid in water
Table 1 Mobile phase gradient elution procedure
Time/min | A (%) | B (%) |
| 0.00 | 10 | 90 |
| 1.5 | 10 | 90 |
| 4 | 100 | 0 |
| 8 | 100 | 0 |
| 8.01 | 10 | 90 |
| 13 | Stop |
Injection volume: 5μL
Column temperature: 30 ° C
Flow rate: 0.3 mL/min
Ion source: electrospray (ESI), positive ion mode detection method: multiple reaction monitoring (MRM)
Table 2 mass spectrometer ion source parameters
Source/Gas | |
| Collision Gas (CAD) | 6 |
| Curtain Gas (CUR) | 30 |
| Ion Source Gas 1 (GS 1) | 50 |
| Ion Source Gas 2 (GS 2) | 50 |
| Ion Spray Voltage(IS) | 5500 |
| Temperature(TEM) | 600 |
| Interface Heater(ihe) | On |
Table 3 Table of parent and daughter ion parameters of aldicarb, aldicarb sulfone and aldicarb sulfoxide
| Substance name | Retention time (min) | Detecting ion pairs | DP | EP | CE | CXP |
| Aldicarb | 7.47 | 208.1/89.1 | 30 | 10 | twenty two | 12 |
| 208.1/116.0 | 30 | 10 | 10 | 12 | ||
| Aldicarb sulfone | 5.86 | 207.1/132.2 | 60 | 10 | 13 | 12 |
| 207.1/89.1 | 60 | 10 | twenty two | 12 | ||
| Aldicarb sulfoxide | 2.86 | 223.1/86.2 | 69 | 10 | twenty one | 12 |
| 223.1/148.1 | 69 | 10 | 13 | 12 |
Seven, the experimental results
1. Ginger base 10μg/kg plus standard recovery results:
The average recovery of the three parallel test samples was greater than 80%, and the relative standard deviations of the parallel samples were less than 5%, which met the standard requirements. (See Table 4)
Table 4 Results of 10μg/kg spiked recovery test in ginger
| name | 1(%) | 2(%) | 3 (%) | The average recovery rate(%) | RSD (%) |
| Aldicarb | 89.23 | 96.74 | 92.86 | 92.94 | 4.05 |
| Aldicarb sulfone | 94.65 | 86.96 | 92.35 | 91.32 | 4.33 |
| Aldicarb sulfoxide | 94.63 | 93.26 | 89.98 | 92.62 | 2.58 |
2. Adding the chromatogram of aldicarb and its metabolites to the blank sample
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