Special issue paper Published online in Wiley Online Library

(wileyonlinelibrary.com) DOI 10.1002/bmc.3092

Analysis of 10 systemic pesticide residues in various baby foods using liquid chromatography–tandem mass spectrometry Angel Yanga, A. M. Abd El-Atya,b*, Jong-Hyouk Parka, Ayman Goudahb, Md. Musfiqur Rahmana, Jung-Ah Doc, Ok-Ja Choid and Jae-Han Shima* ABSTRACT: Ten systemic pesticides, comprising methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazole, and difenoconazole, were detected in 13 baby foods (cereals, boiled potatoes, fruit and milk) using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for sample preparation and liquid chromatography tandem mass spectrometry for analysis. The matrix-matched calibration curves showed good linearity with determination coefficients (R2) > 0.992. The limits of detection and quantitation were 0.0015–0.003 and 0.005–0.01 mg/kg, respectively. The mean recoveries of three different concentrations ranged from 69.2 to 127.1% with relative standard deviations acetone > ACN). EtOAc is more effective than acetone for avoiding sugar coextractives. These solvents provide high pesticide recoveries, but many matrix components are co-extracted. To achieve the required performance characteristics, cleanup techniques such as gel permeation chromatography, solid-phase extraction (SPE) and liquid–liquid partitioning are commonly employed. These procedures lead to increased costs and extended analysis times, and they are labor-intensive (Anastassiades et al., 2003; Park et al., 2011). Various sample preparation methods and types of analytical instrumentation have been reported. For example, Hercegova et al. (2005) developed a sample preparation method based on single-solvent phase extraction and solid-phase extraction (SPE-NH2) cleanup in combination with capillary gas chromatography to detect 18 pesticides of various chemical classes in apples, a common raw material for baby food. In addition, Georgakopoulos et al. (2009) analyzed three nonfat ready-to-eat baby food matrices, fruit juice, fruit puree and fruit cocktail, for pesticide residue using gas chromatography–nitrogen phosphorus detection. Subsequently, they optimized the amount of octadecyl sorbent using the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method to accurately detect organophosphate residues in low-fat baby food (Georgakopoulos et al., 2011). Liquid chromatography (LC) is a more widely used technique than gas chromatography for the analysis of lowvolatility, high-polarity, and thermally labile compounds (Venkateswarlu et al., 2007). LC and/or LC/tandem mass spectrometry (LC-MS/MS) have been used to analyze pesticide residues in baby food samples (Leandro et al., 2006; Gilbert-López et al., 2007, 2012). LC-MS with electrospray or atmosphericpressure chemical ionization has become a critically important tool to quantitatively determine pesticide residues in various matrices in areas such as environmental analysis, food safety and biological exposure monitoring. The LC-MS/MS method has a number of inherent advantages such as high selectivity and sensitivity, simplicity of sample cleanup and ease of accomplishing reliable identification and quantification, even at trace levels (Picó et al., 2006).

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The aim of this study was to develop a selective and sensitive method for analyzing systemic pesticides (five fungicides and five insecticides) in 13 baby foods by LC-MS/MS: methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazole and difenoconazole. These pesticides were selected on the basis of the risk to the consumers.

Experimental Chemicals and materials Pesticide standards were obtained from Dr Ehrenstorfer GmbH (Augsburg, Germany) and Sigma-Aldrich (St Louis, MO, USA; Table 1). Acetic acid (HAc) was supplied by Daejung Chemicals and Materials (Siheung, Republic of Korea) and anhydrous magnesium sulfate (MgSO4) and sodium acetate were purchased from Junsei Chemical Co. Ltd (Kyoto, Japan) and Merck (Darmstadt, Germany). Primary secondary amines and C18 (endcapped) sorbents were obtained from Agilent Technologies (Palo Alto, CA, USA), and analytical-grade ACN and methanol were obtained from Merck.

Preparation of standards Standard stock solutions were prepared by dissolving an appropriate amount of each pesticide in ACN or methanol to yield a concentration of 100 mg/L. Matrix-matched calibration standard solutions were prepared in extracts of fresh samples (containing no target pesticides) purchased from a local market (Gwangju, Republic of Korea) in the limit of quantification (LOQ) range up to 100 × LOQ. All standard solutions were stored at 24°C in dark amber bottles pending analysis.

Sample collection and preparation Representative baby foods were selected based on consumption frequency data reported by the Korea Food and Drug Administration (KFDA, 2008). Thirteen baby foods among the top 30 most frequently consumed by children of ages 0–6 years were selected (Table 2). The selected food samples were obtained from a market-basket survey in Gwangju, Republic of Korea. Milk samples (milk, modified milk powder, soybean milk and yogurt) were collected from two different commercial sources. All food samples were treated in their edible state to estimate health hazards for an actual case. For example, potato and sweet potato were cooked by boiling, and strawberries and milk were tested directly. The cooked samples were homogenized and stored at 21°C pending analysis.

Sample extraction The AOAC QuEChERS method, reported by Lehotay et al. (2005), was employed after minor modifications. Ten grams of homogenized food sample was extracted with 15 mL of ACN containing 150 μL of HAc (pH 5.5–6) in 50 mL Teflon centrifuge tubes. Six grams of anhydrous MgSO4 and 1.5 g of sodium acetate were added and the tubes immediately shaken by hand for 1 min. The extract was then centrifuged at 966g at 4°C for 5 min. A 6 mL aliquot of the extract was transferred to a 15 mL Teflon centrifuge tube containing 900 mg of anhydrous MgSO4 and 300 mg primary secondary amines (+150 mg C18 for fatty food samples – milk, modified milk powder, soybean milk, and yogurt). The Teflon centrifuge tube was shaken by hand for 1 min followed by centrifugation at 966g at 4°C for 5 min. One milliliter of the extract was analyzed by LC-MS/MS.

LC-MS/MS The LC analysis was carried out using a Waters Alliance 2695 Separation Module (Waters Corp., Milford, MA, USA). The chromatographic separation was conducted on a SunFire C18 column (2.1 mm i.d. × 150 mm,

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Analysis of systemic pesticide residues in baby foods Table 1. Liquid chromatography-tandem mass spectroscopy multiple reaction monitoring transition data for the 10 systemic pesticides in baby foods No.

Pesticide

Action

Formula

Retention time (min)

Precursor ion (m/z)

1

Methomyl

Insecticide

C5H10N2O2S

8.431

163.0

2

Thiamethoxam

Insecticide

C8H10ClN5O3S

8.967

292.0

3

Acetamiprid

Insecticide

C10H11ClN4

9.393

223.1

4

Carbofuran

Insecticide

C12H15NO3

10.090

222.1

5

Fosthiazate

Insecticide

C9H18NO3PS2

10.162

284.1

6

Metalaxyl

Fungicide

C15H21NO4

10.233

280.3

7

Azoxystrobin

Fungicide

C22H17N3O5

10.575

404.1

8

Diethofencarb

Fungicide

C14H21NO4

10.647

268.1

9

Propiconazole

Fungicide

C15H17Cl2N3O2

11.099

342.1

10

Difenoconazole

Fungicide

C19H17Cl2N3O3

11.196

406.1

Table 2. Infant food samples for pesticide analysis No.

Food

Form

Group

1 2 3 4 5 6 7 8 9 10 11 12 13

Rice Glutinous rice Potato Sweet potato Apple Banana Strawberry Pear Citrus Milk Modified milk powder Soybean milk Yogurt

Boiled Boiled Boiled Boiled Directly Directly Directly Directly Directly Directly Mixing with water Directly Directly

Cereal grains Potatoes Fruits

Milks

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88.0 106.0 211.0 131.9 121.0 56.0 165.0 123.0 104.0 228.0 220.1 160.1 372.0 344.1 180.0 220.0 69.0 158.8 251.0 111.0

Collision energy (eV) 10 10 12 22 18 18 13 13 12 12 14 14 13 30 20 20 25 25 23 23

Results and discussion Development of LC-MS/MS parameters MS/MS is generally more sensitive than single stage MS for measuring the contents of analytes in complicated matrices because it is associated with higher and more stable signalto-noise (S/N) ratios as a result of specific fragmentations of isolated precursor ions and the elimination of background noise. Protonated molecules, [M + H]+ ions, were observed for all pesticides and were used as precursor ion. In the case of acetamiprid, the intensity of the product ion (qualifier) was minor, and the predominant product ion at m/z 56.003 was used as the quantifying ion to maximize the detection sensitivity of this analyte when present at trace levels. Yeoh and Chong (2012) used m/z 90 as a qualifier ion for the determination of acetamiprid residues in crude palm oil. Despite the low value, Wu et al. (2012) used m/z 56 as a confirmation ion for the determination of acetamiprid in watermelon and soil in an open field. Table 1 shows the LC-MS/MS parameters of the 10 tested pesticides in baby foods. Mobile phase composition can influence ionization performance in the LC-MS/MS method. In the present study, the inclusion of formic acid in the LC solvent improved the signal and the separation of the analytes (Park et al., 2013). Furthermore, ACN provided better chromatographic separation of the tested analytes. A gradient elution program was also selected, as it provided baseline resolution of the analytes with a high detection signal and improved peak shape (Park et al., 2013). The selected program facilitated efficient removal of the matrix constituents, reduced the noise level, and the risk of carry-over effects as well as column deterioration (Park et al., 2013). Filtration of extracts prior to LC-MS/MS analysis is necessary to prevent instrument and column damage, but analyte loss is

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3.5 μm particle size; Waters). Mobile phases A and B consisted of distilled water with 0.1% formic acid (v/v), and ACN with 0.1% formic acid (v/v), respectively. A linear mobile phase gradient program was used as follows: 5% solvent B (0 min), 75% solvent B at 1 min, 95% solvent B at 20 min and 5% solvent B at 30 min. The flow rate and injection volume were set to 0.2 mL/min and 20 μL, respectively. The liquid chromatograph was connected to a Micromass Quattro Micro triple quadrupole mass spectrometer (Waters Corp.), operated in + positive electrospray ionization (ESI ) mode, where all the target + pesticides yielded [M + H] ions. MS/MS detection was conducted using selected reaction monitoring with two mass transitions from the + [M + H] precursor ions. In the two mass transitions, the product ion with the greater intensity and that with the lower intensity were used as quantifier and qualifier ions, respectively (Table 1). The conditions were set as follows: capillary voltage, 3.2 kV; source temperature, 150°C; desolvation temperature, 350°C. The cone and desolvation gases were ultra-pure nitrogen set at flow rates of 30 and 500 L/h, respectively.

Product ion (m/z)

A. Yang et al. commonly encountered owing to adsorption on the membrane filter (Carlson and Thompson, 2000). Based on the findings of Usui et al. (2012) and Park et al. (2013), it is not necessary to consider loss of the analyte when extraction has been carried out using the QuEChERS method, because no problems will occur even if a membrane filter is not used prior to the LC-MS/MS analysis. In addition, because almost all devices used with the QuEChERS method are disposable, there are no issues with potential sample cross-contamination. However, a membrane filter was used prior to LC-MS/MS analysis in this study. The QuEChERS method requires only a simple mixing and centrifugation process. Thus, QuEChERS is cheap, as relatively expensive devices such as SPE vacuum manifolds, pumps and nitrogen evaporators are unnecessary. In addition, little variation is observed in the quantitative values obtained using the QuEChERS method and no statistical outliers are observed

between results obtained by experts and those using the QuEChERs method for the first time (Usui et al., 2012).

Method validation We confirmed that there were no interference peaks at the retention times of the tested analytes by analyzing blank samples (Fig. 1).

Linearity, limit of detection and limit of quantitation Validation studies were carried out with six concentration levels (range from LOQ to LOQ × 2, LOQ × 5, LOQ × 10, LOQ × 20, LOQ × 50, and LOQ × 100) for matrix-matched calibration curves and determination coefficients (R2). The linearity was good with determination coefficients (R2) > 0.992.

Figure 1. Liquid chromatography–tandem mass spectrometry chromatograms of carbofuran (quantifier ion); a blank apple sample (A), in a solvent standard of 0.005 mg/kg (B), a fortified sample of 0.005 mg/kg (C), and actual sample (D).

Table 3. Linearity, limit of detection (LOD), limit of quantification (LOQ) and the lowest maximum residue limits (MRLs) of the target pesticides No.

Compound

1 2 3 4 5 6 7 8 9 10

Methomyl Thiamethoxam Acetamiprid Carbofuran Fosthiazate Metalaxyl Azoxystrobin Diethofencarb Propiconazole Difenoconazole

Linearity (r2) 0.998 0.997 0.994 0.993 0.999 0.992 0.998 0.998 0.999 0.999

LOD (mg/kg) 0.0030 0.0030 0.0030 0.0015 0.0015 0.0015 0.0015 0.0030 0.0025 0.0015

LOQ (mg/kg) 0.010 0.010 0.010 0.005 0.005 0.005 0.005 0.010 0.008 0.005

Lowest MRLa 0.05 0.05 0.10 0.03 0.05 0.05 0.05 0.05 0.05 0.05

a

738

MRLs have established by the KFDA (2011).

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Copyright © 2013 John Wiley & Sons, Ltd.

Azoxystrobin

Diethofencarb

Propiconazole

7

8

9

0.01 0.02 0.1 0.01 0.02 0.1 0.01 0.02 0.1 0.005 0.01 0.05 0.005 0.01 0.05 0.005 0.01 0.05 0.005 0.01 0.05 0.01 0.02 0.1 0.008 0.016 0.08 0.005 0.01 0.05

Fortified concentration (mg/kg)

Milk A and B denote two different companies.

Difenoconazole

Metalaxyl

6

10

Fosthiazate

5

Acetamiprid

3

Carbofuran

Thiamethoxam

2

4

Methomyl

Compound

1

No. 114.4 118.3 117.5 115.6 77.1 90.1 69.0 91.8 94.8 120.4 112.4 107.1 109.9 113.9 98.8 82.6 96.7 111.9 113.9 82.8 115.2 81.6 95.7 93.3 120.2 122.2 111.1 101.8 102.6 93.9

Recovery

Rice

4.5 13.5 9.6 9.1 12.2 13.5 5.1 9.5 12.0 11.0 13.5 10.7 7.5 8.3 2.9 5.4 9.5 4.4 0.2 9.0 6.4 1.1 5.3 6.7 6.6 9.0 0.6 10.0 5.5 2.5

RSD (%) 109.4 106.3 95.4 106.2 95.8 126.1 71.0 102.9 96.6 76.6 83.0 72.4 122.3 115.8 122.2 115.8 72.3 90.2 99.0 94.1 89.0 72.5 80.8 88.1 105.3 118.6 108.0 102.8 111.7 107.6

Recovery 3.5 2.0 7.3 17.5 9.2 9.8 6.0 5.8 4.2 9.3 11.3 5.7 8.5 12.0 2.5 8.1 7.6 0.1 12.0 10.4 7.2 16.9 5.5 7.7 14.6 7.8 1.0 2.3 9.1 2.1

RSD (%)

Potato

111.0 86.6 80.2 94.2 76.4 79.5 99.4 76.6 69.8 69.9 73.1 69.2 125.8 116.4 90.2 103.7 95.1 94.6 90.7 75.9 87.7 70.3 89.2 75.9 87.9 107.7 93.5 84.3 86.7 85.7

Recovery 3.9 5.0 2.9 9.1 3.3 7.0 14.0 0.3 5.3 6.3 10.5 4.0 10.9 9.7 10.9 16.4 4.0 11.5 13.9 3.8 3.8 4.0 10.1 11.6 5.2 5.5 3.2 3.9 4.2 1.8

RSD (%)

Apple

Table 4. Recoveries and relative standard deviations (RSDs) of 10 systemic pesticides in representative baby food samples

115.0 89.0 94.0 94.1 76.9 73.8 113.2 125.1 70.3 81.6 113.5 83.1 92.7 114.0 112.0 87.4 71.6 70.2 102.5 96.8 98.7 99.9 114.0 82.6 88.7 96.3 84.9 77.2 94.8 78.4

Recovery 4.6 5.1 4.9 7.0 7.8 6.5 7.7 4.3 2.3 7.2 15.1 3.9 5.9 5.3 8.4 3.8 10.1 4.6 9.6 3.8 6.9 13.6 8.1 3.2 17.2 4.1 5.4 7.6 6.1 4.7

RSD (%)

A milk

85.7 80.7 98.0 85.1 70.1 84.3 81.4 93.0 76.5 105.0 80.0 107.0 79.8 75.8 107.4 74.1 87.5 82.9 83.5 127.1 71.2 100.6 91.3 114.1 85.3 99.4 87.2 78.8 73.7 82.8

Recovery

2.9 0.5 1.8 4.4 10.3 5.5 7.1 4.3 15.1 5.4 6.7 2.5 3.7 10.5 16.1 3.9 8.4 1.1 11.7 0.6 15.6 4.2 11.4 2.9 9.1 3.1 4.2 11.0 1.9 5.5

RSD (%)

B milk

Analysis of systemic pesticide residues in baby foods

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Matrix effect

172.4 176.4 159.3 109.4 128.8 134.1 68.7 74.5 70.3 81.6 113.5 83.1 73.2 40.4 52.8 131.2 112.3 132.2 71.0 102.9 96.6 76.6 83.0 72.4 69.0 91.8 94.8 120.4 112.4 107.1

120.8 93.2 99.5 89.0 104.1 93.9

SC

99.4 76.6 69.8 69.9 73.1 69.2

182.6 136.4 146.4 90.0 93.7 136.3

The baby foods were spiked in three replicates (n = 3) and mixed with working standard solutions at three different concentrations (LOQ, 2 × LOQ and 10 × LOQ). The fortified samples were allowed to stand to adsorb the analytes onto the samples. The recoveries were 69.2–127.1%, with relative standard deviation values of 0.1–17.5% (Table 4). These results demonstrate that the current method is reliable and reproducible and could be used to analyze pesticides in baby food. The use of a C18 sorbent in fatty baby foods did not affect the recovery of the lipophilic (nonpolar) pesticides, including propiconazole and difenoconazole. This finding contrasts with those of Leandro et al. (2005) and Georgakopoulos et al. (2011). This is because lipophilic molecules may be retained in the lipids removed by the C18 sorbent (Schenck and Wong, 2008).

SC, Recoveries for solvent standard calibration. MC, Recoveries for matrix-matched standard calibration. b

Carbofuran 2

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a

Acetamiprid 1

0.01 0.02 0.1 0.005 0.01 0.05

SC Compound No.

Fortified concentration (mg/kg)

111.4 92.9 93.4 132.5 129.9 115.7

Rice

MC

b

SC

Potato

MC

Apple

MC

SC

A-milk

Recovery

a

Table 5. Comparison of percentage recovery in pure solvent standards and matrix matched standards

The limit of detection (LOD) was determined with a signalto-noise ratio (S/N) ≥ 3, and the LOQ was determined with an S/N ≥ 10: the LODs were 0.0015–0.003 mg/kg, and the LOQs were 0.005–0.01 mg/kg (Table 3). The LOQs were well below the MRL set by the European Commission (Commission Directive 2006/125/EC, 2006). In addition, the LOQ values were lower than those established by the KFDA (2011). Consequently, the method was sufficiently sensitive to analyze pesticides in baby foods.

81.4 96.4 76.5 105.0 80.0 107.0

SC MC

B-milk

MC

A. Yang et al.

The matrix effect, which results in signal suppression or enhancement, depends on the characteristics of the pesticide and matrix as well as the sample treatment procedure (Niessen et al., 2006; Gilbert-López et al., 2007; Kruve et al., 2008). The matrix effect in LC-MS/MS was verified by comparison with solvent standards. The recoveries of representative food samples in solvent standards and matrix-matched standards were compared to evaluate the matrix effect. No substantial differences were observed between the recovery values, except for acetamiprid and carbofuran (Table 5). Therefore, matrixmatched standard calibrations were used to accurately quantify pesticides in various food samples using LC-MS/MS. Method application Commercial baby food samples were collected from local markets in Seoul, Republic of Korea. Milk and yogurt were obtained from three different commercial sources. The 13 samples were analyzed using the QuEChERS method and LC-MS/MS, and none of the tested pesticides were detected in the samples (Fig. 1).

Conclusions The method developed was sensitive and selective, and detected the analytes below the MRL established by the European Commission and the Korea Food and Drug Administration. The combination of QuEChERS sample preparation and LC-MS/MS analysis provided acceptable quantitative and qualitative results in baby food. This method achieved excellent validation results. The foods tested in this study represented some of the most common types consumed raw or with minimal processing by babies. This validation

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Analysis of systemic pesticide residues in baby foods suggests that the method developed here could be used on a wide scale to detect pesticides in various baby foods.

Acknowledgments This study was supported by a grant from The Korea Food and Drug Administration in 2010 (09072 KFDA 997). This paper was also produced with the support of the Ministry of Science, ICT and Future Planning.

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Analysis of 10 systemic pesticide residues in various baby foods using liquid chromatography-tandem mass spectrometry.

Ten systemic pesticides, comprising methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazol...
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